Palladium-Catalyzed Formal (4+2) Cycloaddition between Alkyl Amides and Dienes Initiated by the Activation of C(sp3)‒H Bonds
Cendón, Borja; Font, Marc; Mascareñas, José L.; Gul\?ías, Moisés; ACS Catalysis  (2020) 3425–3430; doi:10.1021/acscatal.0c00664

data_4517447
_publ_section_title
;
 Palladium-Catalyzed Formal (4+2) Cycloaddition between Alkyl Amides and
 Dienes Initiated by the Activation of C(sp3)--H Bonds
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              3425
_journal_page_last               3430
_journal_paper_doi               10.1021/acscatal.0c00664
_journal_year                    2020
_chemical_formula_moiety         '2(C21 H23 N3 O6 Pd S), C H2 Cl2'
_chemical_formula_sum            'C43 H48 Cl2 N6 O12 Pd2 S2'
_chemical_formula_weight         1188.69
_chemical_name_common            'lm1mfm579F(619) - 19MCD00'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                62.2925(14)
_cell_angle_beta                 85.4600(17)
_cell_angle_gamma                73.2316(16)
_cell_formula_units_Z            1
_cell_length_a                   10.6900(5)
_cell_length_b                   11.3617(5)
_cell_length_c                   11.7062(5)
_cell_measurement_reflns_used    9279
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.6844
_cell_measurement_theta_min      2.4569
_cell_volume                     1202.70(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker APEX3 software'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON-III 14'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40696
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.46
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'Incoatec I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.784
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         6479
_refine_ls_number_restraints     1819
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0091P)^2^+1.9711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0757
_reflns_number_gt                5530
_reflns_number_total             6479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00664_si_004.cif
_cod_data_source_block           19MCD007
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 4517447--4517450.cif.
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_cod_database_code               4517447
_shelx_res_checksum              10610
_shelx_hkl_checksum              68081