A neutral diphosphene radical: synthesis, electronic structure and white phosphorus activation.
Haberstroh, Jan; Taube, Clemens; Fidelius, Jannis; Schulz, Stephen; Israel, Noel; Dmitrieva, Evgenia; Gomila, Rosa M.; Frontera, Antonio; Wolf, Robert; Schwedtmann, Kai; Weigand, Jan J.; Chemical communications (Cambridge, England) 60 (2024) 8537–8540; doi:10.1039/d4cc02200a

data_7133304
_publ_section_title
;
 A neutral diphosphene radical: synthesis, electronic structure and white
 phosphorus activation.
;
_journal_issue                   65
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8537
_journal_page_last               8540
_journal_paper_doi               10.1039/d4cc02200a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C39 H51 Cl2 N2 P2'
_chemical_formula_sum            'C39 H51 Cl2 N2 P2'
_chemical_formula_weight         680.66
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2024-04-26 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                86.498(2)
_cell_angle_beta                 73.235(2)
_cell_angle_gamma                66.584(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8940(3)
_cell_length_b                   11.6371(3)
_cell_length_c                   17.3041(2)
_cell_measurement_reflns_used    14700
_cell_measurement_temperature    99.96(12)
_cell_measurement_theta_max      76.6400
_cell_measurement_theta_min      2.6750
_cell_volume                     1923.91(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      99.96(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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    -30.00  10.00   0.50    1.00    --  -38.50  99.00 153.00   80
  2  \w     26.00  72.00   0.50    1.00    --   42.50 -99.00  46.00   92
  3  \w     80.00 107.00   0.50    4.00    --  111.00 -99.00  46.00   54
  4  \w    137.00 178.00   0.50    4.00    --  111.00  99.00 153.00   82
  5  \w   -111.00 -17.00   0.50    1.00    --  -38.50 -38.00   0.00  188
  6  \w   -109.00 -24.00   0.50    1.00    --  -38.50 -38.00  90.00  170
  7  \w     17.00 111.00   0.50    1.00    --   42.50  57.00 -60.00  188
  8  \w     39.00  64.00   0.50    1.00    --   42.50-125.00 -30.00   50
  9  \w     32.00  97.00   0.50    1.00    --   42.50-125.00-120.00  130
 10  \w     72.00  99.00   0.50    4.00    --  111.00-125.00 -60.00   54
 11  \w    107.00 149.00   0.50    4.00    --  111.00 125.00-120.00   84
 12  \w     44.00  72.00   0.50    4.00    --  111.00-125.00   0.00   56
 13  \w    120.00 176.00   0.50    4.00    --  111.00  77.00  60.00  112
 14  \w     38.00  81.00   0.50    4.00    --  111.00 -94.00 120.00   86
 15  \w     42.00  89.00   0.50    4.00    --  111.00-125.00-120.00   94
 16  \w    104.00 144.00   0.50    4.00    --  111.00  77.00 -60.00   80
 17  \w    149.00 177.00   0.50    4.00    --  111.00  77.00 -60.00   56
 18  \w     54.00 107.00   0.50    4.00    --  111.00 -94.00  90.00  106
 19  \w    110.00 135.00   0.50    4.00    --  111.00 -45.00 -60.00   50
 20  \w    104.00 130.00   0.50    4.00    --  111.00  30.00-120.00   52
 21  \w     62.00  89.00   0.50    4.00    --  111.00 -45.00 -60.00   54
 22  \w    102.00 127.00   0.50    4.00    --  111.00-144.00  62.17   50
 23  \w     43.00  88.00   0.50    4.00    --  111.00-144.00  62.17   90
 24  \w     50.00  77.00   0.50    4.00    --  111.00 -61.00-120.00   54
 25  \w     94.00 138.00   0.50    4.00    --  111.00 -61.00-120.00   88
 26  \w     66.00 177.00   0.50    4.00    --  111.00  15.00-150.00  222
 27  \w     30.00 104.00   0.50    4.00    --  111.00 -94.00  60.00  148
 28  \w     75.00 125.00   0.50    4.00    --  111.00-142.00   2.18  100
 29  \w     40.00 112.00   0.50    4.00    --  111.00-125.00 -90.00  144
 30  \w     31.00 107.00   0.50    4.00    --  111.00 -94.00   0.00  152
 31  \w    116.00 143.00   0.50    4.00    --  111.00  77.00  30.00   54
 32  \w     70.00 106.00   0.50    4.00    --  111.00 -94.00 150.00   72
 33  \w     41.00  83.00   0.50    4.00    --  111.00 -61.00 120.00   84
 34  \w     41.00 120.00   0.50    4.00    --  111.00-136.00 -55.75  158
 35  \w    102.00 178.00   0.50    4.00    --  111.00  45.00  90.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1080662000
_diffrn_orient_matrix_UB_12      -0.0434660000
_diffrn_orient_matrix_UB_13      -0.0149310000
_diffrn_orient_matrix_UB_21      -0.0943853000
_diffrn_orient_matrix_UB_22      0.0478421000
_diffrn_orient_matrix_UB_23      0.0866581000
_diffrn_orient_matrix_UB_31      -0.0729129000
_diffrn_orient_matrix_UB_32      0.1292742000
_diffrn_orient_matrix_UB_33      -0.0307429000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21226
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.290
_diffrn_reflns_theta_min         2.672
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.508
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.188
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.545
_exptl_crystal_size_mid          0.441
_exptl_crystal_size_min          0.377
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         8000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0645P)^2^+1.1438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7878
_reflns_number_total             8000
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02200a2.cif
_cod_data_source_block           jjw1231
_cod_depositor_comments
'Adding full bibliography for 7133304--7133306.cif.'
_cod_database_code               7133304
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C72 H102 Cl4 N10 S4 P1 '
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Ternary CH refined with riding coordinates:
 C3(H3), C10(H10), C16(H16), C23(H23), C30(H30), C37(H37)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C19(H19), C20(H20), C21(H21), C33(H33), C34(H34),
 C35(H35)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C)
;
_shelx_res_checksum              57299
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.377
_oxdiff_exptl_absorpt_empirical_full_min 0.787