Harnessing Secondary Coordination Sphere Interactions That Enable the Selective Amidation of Benzylic C-H Bonds.
Jung, Hoimin; Schrader, Malte; Kim, Dongwook; Baik, Mu-Hyun; Park, Yoonsu; Chang, Sukbok; Journal of the American Chemical Society 141 (2019) 15356–15366; doi:10.1021/jacs.9b07795

data_4128964
_publ_section_title
;
 Harnessing Secondary Coordination Sphere Interactions That Enable the
 Selective Amidation of Benzylic C-H Bonds.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15356
_journal_page_last               15366
_journal_paper_doi               10.1021/jacs.9b07795
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C19 H15 F6 N4 O2 P Ru'
_chemical_formula_weight         577.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7237(10)
_cell_length_b                   13.3153(13)
_cell_length_c                   13.7472(13)
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      29.01
_cell_measurement_theta_min      3.06
_cell_volume                     2146.0(3)
_computing_cell_refinement       'Bruker APEXIII'
_computing_data_collection       'Bruker APEXIII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62687
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.203
_diffrn_reflns_theta_min         3.335
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.882
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.7004
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_description       rod
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1782 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.006(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5780
_refine_ls_number_restraints     595
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0376P)^2^+1.4684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4688
_reflns_number_total             5780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07795_si_002.cif
_cod_data_source_block           A079_019
_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/current/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 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4128964
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              43218
_shelx_hkl_checksum              37861