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_7034116
_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         'C27 H30 N2 O3 Pd,0.75 C6 H14'
_chemical_formula_sum            'C31.5 H40.5 N2 O3 Pd'
_chemical_formula_weight         601.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 110.788(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.910(8)
_cell_length_b                   14.159(4)
_cell_length_c                   15.463(5)
_cell_measurement_reflns_used    847
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.322
_cell_measurement_theta_min      2.349
_cell_volume                     5508(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0834
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21197
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.579
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 7716 reflections(SADABS);Rint 0.0758 before
correction and 0.0515 after.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2508
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
Disordered C6H14 was omitted using the SQUEEZE option of PLATON.The solvent
accessible voids are 954.4 \%A3 with an estimated 316e/cell to be added.Six
solvent C6H14 molecules/unit cell accounting for 300e 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         1.092
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.959
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         5402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.959
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0476P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                3979
_reflns_number_total             5402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5dt00062a1.cif
_cod_data_source_block           11004
_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      C2/c
_cod_original_formula_sum        'C31.50 H40.50 N2 O3 Pd'
_cod_database_code               7034116