The ortho effect in directed C‒H activation
Tóth, Balázs L.; Monory, Anna; Egyed, Orsolya; Domján, Attila; Bényei, Attila; Szathury, Bálint; Novák, Zoltán; Stirling, András; Chemical Science 12 (2021) 5152–5163; doi:10.1039/D1SC00642H

data_1560760
_publ_section_title
;
 The ortho effect in directed C--H activation
;
_journal_issue                   14
_journal_name_full               'Chemical Science'
_journal_page_first              5152
_journal_page_last               5163
_journal_paper_doi               10.1039/D1SC00642H
_journal_volume                  12
_journal_year                    2021
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C32 H24 F6 N2 O6 Pd2, C3 H6 O'
_chemical_formula_sum            'C35 H30 F6 N2 O7 Pd2'
_chemical_formula_weight         917.41
_chemical_name_common            MA28
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-11-16 deposited with the CCDC.	2021-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.712(6)
_cell_length_b                   13.024(2)
_cell_length_c                   15.254(3)
_cell_measurement_reflns_used    314
_cell_measurement_temperature    298.(2)
_cell_measurement_theta_max      32.3799
_cell_measurement_theta_min      2.1147
_cell_volume                     7492(2)
_computing_cell_refinement       'APEX3 v2017.3-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.6'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    Mercury
_computing_publication_material  'WinGX, PublCIF'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.(2)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \p scan'
_diffrn_radiation_monochromator  'multilayer mirror INCOATEC'
_diffrn_radiation_type           ' Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16999
_diffrn_reflns_theta_full        25.39
_diffrn_reflns_theta_max         25.39
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              'INCOATEC I\mS 3.0'
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.74
_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    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.520
_refine_ls_abs_structure_details
;

Flack x determined using 747 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         3350
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0512
_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^)+(0.0627P)^2^+3.5573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1377
_reflns_number_gt                2121
_reflns_number_total             3350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00642h5.cif
_cod_data_source_block           9_Pd
_cod_depositor_comments
'Adding full bibliography for 1560759--1560764.cif.'
_cod_original_cell_volume        7492.(2)
_cod_database_code               1560760
_publcif_datablock.id            {72039a91-1373-4dff-9846-45d45dcfeee4}
_shelx_res_checksum              4945
_shelx_hkl_checksum              53301