Understanding Regiodivergence in a Pd(II)-Mediated Site-Selective C‒H Alkynylation
Usui, Kenji; Haines, Brandon E.; Musaev, Djamaladdin G.; Sarpong, Richmond; ACS Catalysis 8 (2018) 4516–; doi:10.1021/acscatal.8b01116

data_4515575
_publ_section_title
;
 Understanding Regiodivergence in a Pd(II)-Mediated Site-Selective C--H
 Alkynylation
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4516
_journal_paper_doi               10.1021/acscatal.8b01116
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C25 H25 N3 O Pd'
_chemical_formula_weight         489.88
_chemical_name_common            KU2_011
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.171(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5510(7)
_cell_length_b                   9.9456(5)
_cell_length_c                   17.6307(9)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      2.33
_cell_volume                     2113.72(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.417
_diffrn_reflns_theta_min         1.780
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       Block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         1.946
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0066P)^2^+7.9535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0682
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3432
_reflns_number_total             3892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b01116_si_002.cif
_cod_data_source_block           KU2_011
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515575
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.877
_shelx_res_checksum              1135
_shelx_hkl_checksum              3634