Mechanochemical C-H bond activation: rapid and regioselective double cyclopalladation monitored by in situ Raman spectroscopy
Marina Juribasic; Krunoslav Uzarevic; Davor Gracin; Manda Curic; Chem.Commun. 50 (2014) 10287–; doi:10.1039/C4cc04423A

data_7115539
_publ_section_title
;
 Mechanochemical C-H bond activation: rapid and regioselective double
 cyclopalladation monitored by in situ Raman spectroscopy
;
_journal_name_full               Chem.Commun.
_journal_page_first              10287
_journal_paper_doi               10.1039/C4cc04423A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C36 H36 N8 O12 Pd4, 2(C4 H8 O1)'
_chemical_formula_sum            'C44 H52 N8 O14 Pd4'
_chemical_formula_weight         1342.54
_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'
_audit_creation_date             2014-05-05T17:03:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.124(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9571(3)
_cell_length_b                   23.6001(8)
_cell_length_c                   13.0293(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2445.07(16)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
        (compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10294
_diffrn_reflns_theta_full        27
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_min         4.3
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.558
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5247
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+1.8454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                3909
_reflns_number_total             5247
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc04423a2.cif
_cod_data_source_block           exp_2904
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7115539