Product inhibition in nucleophilic aromatic substitution through DPPPent-supported π-arene catalysis.
Mueller, Benjamin R. J.; Schley, Nathan D.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 10114–10119; doi:10.1039/d0dt00786b

data_7704777
_publ_section_title
;
 Product inhibition in nucleophilic aromatic substitution through
 DPPPent-supported \p-arene catalysis.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10114
_journal_page_last               10119
_journal_paper_doi               10.1039/d0dt00786b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C35 H34 F P2 Ru, C F3 O3 S'
_chemical_formula_sum            'C36 H34 F4 O3 P2 Ru S'
_chemical_formula_weight         785.70
_chemical_properties_physical    Air-sensitive
_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     dual
_audit_creation_date             2018-12-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-10-22 deposited with the CCDC.	2020-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3482(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.85714(20)
_cell_length_b                   9.81404(12)
_cell_length_c                   30.3186(3)
_cell_measurement_reflns_used    14059
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.9080
_cell_measurement_theta_min      2.9120
_cell_volume                     6484.83(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -108.00  -8.00   1.00    8.00    --  -37.09 -19.00  90.00  100
  2  \w    -64.00  30.00   1.00    8.00    --  -37.09  77.00   0.00   94
  3  \w   -104.00 -20.00   1.00    8.00    --  -37.09 -57.00 -90.00   84
  4  \w   -104.00 -20.00   1.00    8.00    --  -37.09 -57.00-150.00   84
  5  \w    -54.00  30.00   1.00    8.00    --  -37.09  57.00 -90.00   84
  6  \w      1.00  76.00   1.00    8.00    --   37.09 -99.00 -30.00   75
  7  \w      1.00  76.00   1.00    8.00    --   37.09 -99.00  60.00   75
  8  \w     20.00 104.00   1.00    8.00    --   37.09  57.00 120.00   84
  9  \w     23.00  90.00   1.00    8.00    --   37.09-125.00 -90.00   67
 10  \w     20.00 104.00   1.00    8.00    --   37.09  57.00-120.00   84
 11  \w     57.00 150.00   1.00   30.00    --  111.00 178.00 150.00   93
 12  \w     90.00 178.00   1.00   30.00    --  111.00  30.00 -60.00   88
 13  \w     42.00 109.00   1.00   30.00    --  111.00 -94.00 -60.00   67
 14  \w     93.00 178.00   1.00   30.00    --  111.00  61.00  60.00   85
 15  \w     84.00 178.00   1.00   30.00    --  111.00  77.00   0.00   94
 16  \w     94.00 178.00   1.00   30.00    --  111.00  45.00-180.00   84
 17  \w     43.00 138.00   1.00   30.00    --  111.00 -77.00-120.00   95
 18  \w     93.00 178.00   1.00   30.00    --  111.00  61.00 -30.00   85
 19  \w     44.00  62.00   1.00   30.00    --  111.00 -61.00   0.00   18
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0189499000
_diffrn_orient_matrix_UB_12      0.1115428000
_diffrn_orient_matrix_UB_13      0.0340999000
_diffrn_orient_matrix_UB_21      -0.0129560000
_diffrn_orient_matrix_UB_22      -0.0981409000
_diffrn_orient_matrix_UB_23      0.0378384000
_diffrn_orient_matrix_UB_31      0.0668319000
_diffrn_orient_matrix_UB_32      -0.0507380000
_diffrn_orient_matrix_UB_33      0.0017115000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            42422
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.408
_diffrn_reflns_theta_min         2.408
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.970
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane, THF'
_exptl_crystal_size_max          0.124
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.037
_refine_diff_density_max         1.823
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     884
_refine_ls_number_reflns         12620
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+10.8594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1149
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10264
_reflns_number_total             12620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00786b3.cif
_cod_data_source_block           complex_1
_cod_depositor_comments
'Adding full bibliography for 7704777--7704780.cif.'
_cod_original_cell_volume        6484.84(12)
_cod_database_code               7704777
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C36H34F4O3P2RuS
_reflns_odcompleteness_completeness 98.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
F2B \\sim F2C \\sim F3B \\sim F3C \\sim F4B \\sim F4C \\sim C36B \\sim C36C:
within 1.5A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(F2C)=Sof(F3C)=Sof(F4C)=Sof(C36C)=1-FVAR(1)
 Sof(F2B)=Sof(F3B)=Sof(F4B)=Sof(C36B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C9(H9), C9B(H9B)
4.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C7B(H7BA,H7BB),
 C8B(H8BA,H8BB), C10B(H10C,H10D), C11B(H11C,H11D)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
 C34(H34), C35(H35), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B), C19B(H19B),
 C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C25B(H25B), C26B(H26B),
 C27B(H27B), C28B(H28B), C29B(H29B), C31B(H31B), C32B(H32B), C33B(H33B),
 C34B(H34B), C35B(H35B)
;
_shelx_res_checksum              90161
_olex2_date_sample_data_collection 2018-12-05
_olex2_exptl_crystal_mounting_method 'mounted in a polyimide loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.082
_oxdiff_exptl_absorpt_empirical_full_min 0.932