N,N-Chelate-control on the regioselectivity in acetate-assisted C-H activation.
Cross, Warren B.; Hope, Eric G.; Lin, Yi-Hsien; Macgregor, Stuart A.; Singh, Kuldip; Solan, Gregory A.; Yahya, Nurhusna; Chemical communications (Cambridge, England) 49 (2013) 1918–1920; doi:10.1039/c3cc38697j

data_7112442
_publ_section_title
;
 N,N-Chelate-control on the regioselectivity in acetate-assisted C-H
 activation.
;
_journal_issue                   19
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1918
_journal_page_last               1920
_journal_paper_doi               10.1039/c3cc38697j
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C32 H36 N2 O2 Pd,1.5 H2 O'
_chemical_formula_sum            'C32 H39 N2 O3.5 Pd'
_chemical_formula_weight         614.05
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.929(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.965(3)
_cell_length_b                   15.135(5)
_cell_length_c                   20.959(7)
_cell_measurement_reflns_used    819
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.458
_cell_measurement_theta_min      2.363
_cell_volume                     2843.5(16)
_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  0.1215
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21814
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absorption correction based on 7089 reflections(SADABS);Rint 0.1099 before
correction and 0.0456 after.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.576
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         5568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                4031
_reflns_number_total             5568
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7108900
_cod_data_source_file            c3cc38697j.txt
_cod_data_source_block           12069
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/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_cell_volume        2843.6(16)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C32 H39 N2 O3.50 Pd'
_cod_database_code               7112442