Triplet quenching pathway control with molecular dyads enables the identification of a highly oxidizing annihilator class.
Bertrams, Maria-Sophie; Hermainski, Katharina; Mörsdorf, Jean-Marc; Ballmann, Joachim; Kerzig, Christoph; Chemical science 14 (2023) 8583–8591; doi:10.1039/d3sc01725g

data_1569550
_publ_section_title
;
 Triplet quenching pathway control with molecular dyads enables the
 identification of a highly oxidizing annihilator class.
;
_journal_issue                   32
_journal_name_full               'Chemical science'
_journal_page_first              8583
_journal_page_last               8591
_journal_paper_doi               10.1039/d3sc01725g
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '2(C26 H34 Cl2 P2), 4(Cl), 3(H2 O)'
_chemical_formula_sum            'C52 H74 Cl8 O3 P4'
_chemical_formula_weight         1154.59
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-06 deposited with the CCDC.	2023-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                78.259(4)
_cell_angle_beta                 76.680(4)
_cell_angle_gamma                69.650(5)
_cell_formula_units_Z            2
_cell_length_a                   11.9371(8)
_cell_length_b                   15.3069(7)
_cell_length_c                   17.4558(6)
_cell_measurement_reflns_used    13246
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      32.2030
_cell_measurement_theta_min      2.6220
_cell_volume                     2883.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.51a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.948
_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    -55.00  45.00   0.50   30.00    --  -25.00  77.00 -90.00  200
  2  \w    -41.00  57.00   0.50   30.00    --   31.15 -38.00   0.00  196
  3  \w    -20.00  73.00   0.50   30.00    --   31.15 -99.00 150.00  186
  4  \w    -41.00  57.00   0.50   30.00    --   31.15 -38.00 150.00  196
  5  \w      1.00 101.00   0.50   30.00    --   31.15  77.00-120.00  200
  6  \w    -20.00  73.00   0.50   30.00    --   31.15 -99.00  60.00  186
  7  \w    -20.00  73.00   0.50   30.00    --   31.15 -99.00-180.00  186
  8  \w    -20.00  73.00   0.50   30.00    --   31.15 -99.00 -60.00  186
  9  \w     11.00 100.00   0.50   30.00    --   31.15  57.00   0.00  178
 10  \w      6.00 104.00   0.50   30.00    --   31.15  38.00 150.00  196
 11  \w    -20.00  73.00   0.50   30.00    --   31.15 -99.00   0.00  186
 12  \w      6.00 104.00   0.50   30.00    --   31.15  38.00 -60.00  196
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0592212000
_diffrn_orient_matrix_UB_12      0.0021915000
_diffrn_orient_matrix_UB_13      -0.0029506000
_diffrn_orient_matrix_UB_21      0.0239547000
_diffrn_orient_matrix_UB_22      -0.0224278000
_diffrn_orient_matrix_UB_23      -0.0347024000
_diffrn_orient_matrix_UB_31      0.0077914000
_diffrn_orient_matrix_UB_32      -0.0445011000
_diffrn_orient_matrix_UB_33      0.0237319000
_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  0.0886
_diffrn_reflns_av_unetI/netI     0.0954
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            92290
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.155
_diffrn_reflns_theta_min         2.378
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.745
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.51a (Rigaku Oxford Diffraction, 2022)
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    1.330
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         22576
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1079
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0387P)^2^+0.1284P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14083
_reflns_number_total             22576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01725g2.cif
_cod_data_source_block           ba_para_chloro
_cod_depositor_comments
'Adding full bibliography for 1569549--1569550.cif.'
_cod_database_code               1569550
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H63E-O63 \\sim O63-H63D
 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C21(H21), C24(H24), C38(H38), C41(H41), C58(H58), C61(H61)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C11(H11), C13(H13), C14(H14), C34(H34), C36(H36),
 C37(H37), C54(H54), C56(H56), C57(H57)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              93857
_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 1.366
_oxdiff_exptl_absorpt_empirical_full_min 0.736