Photoexcited Pd(ii) auxiliaries enable light-induced control in C(sp3)‒H bond functionalisation
Czyz, Milena L.; Weragoda, Geethika K.; Horngren, Tyra H.; Connell, Timothy U.; Gomez, Daniel; O'Hair, Richard A. J.; Polyzos, Anastasios; Chemical Science 11 (2020) 2455–2463; doi:10.1039/C9SC05722F

data_1557142
_publ_section_title
;
 Photoexcited Pd(ii) auxiliaries enable light-induced control in C(sp3)--H
 bond functionalisation
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              2455
_journal_page_last               2463
_journal_paper_doi               10.1039/C9SC05722F
_journal_volume                  11
_journal_year                    2020
_chemical_formula_sum            'C18 H20 Cl N3 O Pd'
_chemical_formula_weight         436.22
_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
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-11-12 deposited with the CCDC.	2020-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                70.420(4)
_cell_angle_beta                 78.131(4)
_cell_angle_gamma                84.462(4)
_cell_formula_units_Z            2
_cell_length_a                   7.5074(4)
_cell_length_b                   11.2005(6)
_cell_length_c                   11.2581(5)
_cell_measurement_reflns_used    7049
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      35.3450
_cell_measurement_theta_min      2.7640
_cell_volume                     872.46(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.95(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19203
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.213
_diffrn_reflns_theta_min         2.774
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.580
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, hexane'
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.016
_refine_diff_density_max         1.720
_refine_diff_density_min         -2.367
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         8018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0686
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0503P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6236
_reflns_number_total             8018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc05722f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;Adding full bibliography for 1557142.cif.

 Adding full bibliography for 1557142.cif.
;
_cod_database_code               1557142
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment     'Tyra Horngren Pd complex'
_oxdiff_exptl_absorpt_empirical_full_min 0.725
_oxdiff_exptl_absorpt_empirical_full_max 2.086
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              63556