Aerobic C‒H Acetoxylation of 8-Methylquinoline in PdII‒Pyridinecarboxylic Acid Systems: Some Structure‒Reactivity Relationships
Wang, Daoyong; Zavalij, Peter Y.; Vedernikov, Andrei N.; Organometallics 32 (2013) 4882–; doi:10.1021/om400618n

data_4081341
_publ_section_title
;
 Aerobic C--H Acetoxylation of 8-Methylquinoline in
 PdII--Pyridinecarboxylic Acid Systems: Some Structure--Reactivity
 Relationships
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4882
_journal_paper_doi               10.1021/om400618n
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         '2(C22 H22 N2 O4 Pd), C4 H10 O, 4(C2 H4 O2)'
_chemical_formula_sum            'C56 H70 N4 O17 Pd2'
_chemical_formula_weight         1283.96
_chemical_name_common            Pd-complex
_chemical_name_systematic
;
Pd-complex
;
_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 & ZCIF'
_cell_angle_alpha                111.3499(19)
_cell_angle_beta                 92.9602(19)
_cell_angle_gamma                98.317(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4534(17)
_cell_length_b                   15.2917(19)
_cell_length_c                   15.3176(19)
_cell_measurement_reflns_used    16576
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.2
_cell_volume                     2885.4(6)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      610,610,610,900
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0547912
_diffrn_orient_matrix_UB_12      0.0038372
_diffrn_orient_matrix_UB_13      -0.0497321
_diffrn_orient_matrix_UB_21      0.0517427
_diffrn_orient_matrix_UB_22      0.0074997
_diffrn_orient_matrix_UB_23      -0.0383244
_diffrn_orient_matrix_UB_31      -0.0060801
_diffrn_orient_matrix_UB_32      -0.0700431
_diffrn_orient_matrix_UB_33      -0.0338377
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30216
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.17
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.895
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_id                'Vedern/Wang wdy-1 in HAc Et2O 100K'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.255
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.408
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     815
_refine_ls_number_reflns         10144
_refine_ls_number_restraints     563
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+18.P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                8301
_reflns_number_total             10144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400618n_si_002.cif
_cod_data_source_block           2004
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081341
_diffrn_measurement_frame_width-ccd -0.30
_diffrn_measurement_total_frames-ccd 2730
_diffrn_measurement_frame_time-ccd 25
_diffrn_measurement_total_time-ccd 23.5
_diffrn_detector_distance-ccd    5.000
_diffrn_measurement_frame_size-ccd 512