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_4517450
_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         'C25 H25 Cl2 N3 O Pd'
_chemical_formula_sum            'C25 H25 Cl2 N3 O Pd'
_chemical_formula_weight         560.78
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2018/3
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_cell_angle_beta                 105.716(17)
_cell_angle_gamma                105.330(16)
_cell_formula_units_Z            2
_cell_length_a                   9.0308(5)
_cell_length_b                   11.8072(6)
_cell_length_c                   11.9867(6)
_cell_measurement_reflns_used    9180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.49
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_cell_volume                     1156.3(2)
_computing_cell_refinement       'BRUKER APEX3'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON III-14'
_diffrn_measurement_method       'omega and phi'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
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_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            88190
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS-2016/2'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.180
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_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.7764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10210
_reflns_number_total             11205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c00664_si_006.cif
_cod_data_source_block           complex_6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

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

 Adding full bibliography for 4517447--4517450.cif.
;
_cod_original_cell_volume        1156.32(2)
_cod_database_code               4517450
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.833
_shelx_estimated_absorpt_t_max   0.930
_shelx_res_checksum              30864
_shelx_hkl_checksum              64686