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_7704778
_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         'C46 H45 P2 Ru, C F3 O3 S, C4 H10 O'
_chemical_formula_sum            'C51 H55 F3 O4 P2 Ru S'
_chemical_formula_weight         984.02
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-02 deposited with the CCDC.	2020-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.19031(12)
_cell_length_b                   19.05235(16)
_cell_length_c                   29.7018(3)
_cell_measurement_reflns_used    21323
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.2940
_cell_measurement_theta_min      2.9680
_cell_volume                     9161.92(14)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1506
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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   -104.00 -20.00   1.00    3.00    --  -37.09 -57.00-150.00   84
  2  \w    -56.00  32.00   1.00    3.00    --  -37.09  38.00-180.00   88
  3  \w    -30.00  64.00   1.00    3.00    --   37.09 -77.00-150.00   94
  4  \w    -30.00  54.00   1.00    3.00    --   37.09 -57.00  30.00   84
  5  \w    -30.00  64.00   1.00    3.00    --   37.09 -77.00 -90.00   94
  6  \w     20.00 104.00   1.00    3.00    --   37.09  57.00   0.00   84
  7  \w     41.00 132.00   1.00   10.00    --  111.00 -30.00-150.00   91
  8  \w     43.00 138.00   1.00   10.00    --  111.00 -77.00-180.00   95
  9  \w     41.00 132.00   1.00   10.00    --  111.00 -30.00  30.00   91
 10  \w     41.00 132.00   1.00   10.00    --  111.00 -30.00 -60.00   91
 11  \w     44.00 129.00   1.00   10.00    --  111.00 -61.00-120.00   85
 12  \w     44.00 129.00   1.00   10.00    --  111.00 -61.00   0.00   85
 13  \w   -105.00 -47.00   1.00    3.00    --  -37.09 -77.00  60.00   58
 14  \w   -104.00 -20.00   1.00    3.00    --  -37.09 -57.00 120.00   84
;
_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      -0.0078449000
_diffrn_orient_matrix_UB_12      -0.0092791000
_diffrn_orient_matrix_UB_13      -0.0513690000
_diffrn_orient_matrix_UB_21      -0.0910987000
_diffrn_orient_matrix_UB_22      -0.0216393000
_diffrn_orient_matrix_UB_23      0.0057255000
_diffrn_orient_matrix_UB_31      -0.0263939000
_diffrn_orient_matrix_UB_32      0.0773173000
_diffrn_orient_matrix_UB_33      -0.0044998000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            46582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.426
_diffrn_reflns_theta_min         2.976
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.328
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.563
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       plate
_exptl_crystal_F_000             4080
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Methanol/Et2O'
_exptl_crystal_size_max          0.195
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.865
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     567
_refine_ls_number_reflns         9125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+21.8696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8207
_reflns_number_total             9125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00786b3.cif
_cod_data_source_block           complex_4-OTf
_cod_depositor_comments
'Adding full bibliography for 7704777--7704780.cif.'
_cod_original_cell_volume        9161.92(13)
_cod_database_code               7704778
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C51H55F3O4P2RuS
_reflns_odcompleteness_completeness 99.97
_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
 At 1.5 times of:
  All C(H,H,H) groups
 At 1.7 times of:
  All Ru(H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C12(H12), C13(H13), C14(H14), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
  C26(H26), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C48(H48A,H48B,H48C),
 C51(H51A,H51B,H51C)
;
_shelx_res_checksum              35715
_olex2_date_sample_data_collection 2019-10-29
_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 1.120
_oxdiff_exptl_absorpt_empirical_full_min 0.900