O,N,N-Pincer ligand effects on oxidatively induced carbon-chlorine coupling reactions at palladium.
Wright, Luka A.; Hope, Eric G.; Solan, Gregory A.; Cross, Warren B.; Singh, Kuldip; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6040–6051; doi:10.1039/c5dt00062a

data_7034117
_publ_section_title
;
 O,N,N-Pincer ligand effects on oxidatively induced carbon-chlorine
 coupling reactions at palladium.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6040
_journal_page_last               6051
_journal_paper_doi               10.1039/c5dt00062a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C25 H28 N2 O3 Pd, 1.5 C H Cl3'
_chemical_formula_sum            'C26.5 H29.5 Cl4.5 N2 O3 Pd'
_chemical_formula_weight         689.95
_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
;
2015-02-09 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.643(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.155(4)
_cell_length_b                   13.910(3)
_cell_length_c                   13.360(3)
_cell_measurement_reflns_used    681
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.568
_cell_measurement_theta_min      2.929
_cell_volume                     2827.5(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1884
_diffrn_reflns_av_sigmaI/netI    0.3022
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22017
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 2191 reflections(SADABS);Rint 0.0830 before
correction and 0.0505 after.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
Disordered CHCl3 was omitted using the SQUEEZE option of PLATON.The solvent
accessible voids are 864.5 \%A3 with an estimated 385e/cell to be added.Six solvent 
CHCl3 molecules/unit cell accounting for 348e were included in the formula, FWt, 
(000) and density calculations. PLATON Reference: Spek, A.L. (1990),
Acta Cryst. A46, C-34.   
;
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.725
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5551
_refine_ls_number_restraints     277
_refine_ls_restrained_S_all      0.714
_refine_ls_R_factor_all          0.1940
_refine_ls_R_factor_gt           0.0695
_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^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                1647
_reflns_number_total             5551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00062a1.cif
_cod_data_source_block           13083
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7034115--7034122.cif.
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C26.50 H29.50 Cl4.50 N2 O3 Pd'
_cod_database_code               7034117