Reactivity of ketenyl anions towards ammonia.
Duari, Prakash; Jörges, Mike; Mondal, Sunita; Feichtner, Kai-Stephan; Gessner, Viktoria H.; Chemical communications (Cambridge, England) 62 (2026) 4293–4297; doi:10.1039/d5cc06975k

data_7135428
_publ_section_title
;
 Reactivity of ketenyl anions towards ammonia.
;
_journal_issue                   14
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4293
_journal_page_last               4297
_journal_paper_doi               10.1039/d5cc06975k
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C28 H25 N O2 P2 S2'
_chemical_formula_sum            'C28 H25 N O2 P2 S2'
_chemical_formula_weight         533.55
_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             2024-12-02
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-11-25 deposited with the CCDC.	2026-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.1780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0525(2)
_cell_length_b                   9.02100(10)
_cell_length_c                   22.2487(3)
_cell_measurement_reflns_used    18949
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.8230
_cell_measurement_theta_min      3.6460
_cell_volume                     2570.01(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_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    -59.00  22.00   0.50    1.00    --  -47.28  60.00 -60.00  162
  2  \w   -118.00 -35.00   0.50    1.00    --  -47.28 -60.00 160.00  166
  3  \w    -15.00  29.00   0.50    1.00    --   47.28 -60.00 160.00   88
  4  \w     70.00  96.00   0.50    1.00    --   47.28  60.00 -60.00   52
  5  \w   -163.00-121.00   0.50    4.00    --  -91.75 -60.00 160.00   84
  6  \w    -67.00 -42.00   0.50    4.00    --  -91.75  60.00 -60.00   50
  7  \w    126.00 174.00   0.50    4.00    --  105.91  60.00 -60.00   96
  8  \w     34.00  66.00   0.50    4.00    --  105.91 -60.00 160.00   64
  9  \w    -16.00  28.00   0.50    1.00    --  -47.28  19.00  60.00   88
 10  \w   -117.00 -85.00   0.50    1.00    --  -47.28-125.00 -90.00   64
 11  \w   -100.00 -73.00   0.50    1.00    --  -47.28-125.00 120.00   54
 12  \w    -83.00 -33.00   0.50    1.00    --  -47.28 125.00-180.00  100
 13  \w    -27.00  28.00   0.50    1.00    --   47.28 -19.00-180.00  110
 14  \w   -159.00 -79.00   0.50    4.00    --  -91.75 -45.00  30.00  160
 15  \w    -64.00 -21.00   0.50    4.00    --  -91.75 125.00 -30.00   86
 16  \w    -59.00 -21.00   0.50    4.00    --  -91.75  61.00 120.00   76
 17  \w   -153.00 -80.00   0.50    4.00    --  -91.75 -30.00 -60.00  146
 18  \w    -47.00 -21.00   0.50    4.00    --  -91.75  45.00 -60.00   52
 19  \w    -48.00 -22.00   0.50    4.00    --  -91.75  45.00  30.00   52
 20  \w    -84.00 -21.00   0.50    4.00    --  -91.75  77.00 120.00  126
 21  \w    -48.00 -23.00   0.50    4.00    --  -91.75  45.00  60.00   50
 22  \w     93.00 177.00   0.50    4.00    --  105.91  45.00-120.00  168
 23  \w     79.00 105.00   0.50    4.00    --  105.91 -94.00   0.00   52
 24  \w     42.00  93.00   0.50    4.00    --  105.91 -77.00 -30.00  102
 25  \w     66.00  92.00   0.50    4.00    --  105.91 -94.00-180.00   52
 26  \w     46.00 112.00   0.50    4.00    --  105.91-125.00 -60.00  132
 27  \w     92.00 178.00   0.50    4.00    --  105.91  61.00-150.00  172
 28  \w     77.00 103.00   0.50    4.00    --  105.91 -94.00-150.00   52
 29  \w     43.00  68.00   0.50    4.00    --  105.91 -94.00-150.00   50
 30  \w     33.00  65.00   0.50    4.00    --  105.91 -94.00-180.00   64
 31  \w     39.00 106.00   0.50    4.00    --  105.91 -94.00 120.00  134
 32  \w     77.00 106.00   0.50    4.00    --  105.91-101.00  94.33   58
 33  \w     93.00 178.00   0.50    4.00    --  105.91  45.00 150.00  170
 34  \w     41.00 109.00   0.50    4.00    --  105.91-125.00 -30.00  136
 35  \w     46.00  84.00   0.50    4.00    --  105.91 -94.00  60.00   76
 36  \w     49.00  75.00   0.50    4.00    --  105.91-112.00 -64.87   52
 37  \w     83.00 108.00   0.50    4.00    --  105.91-112.00 -64.87   50
 38  \w     39.00 104.00   0.50    4.00    --  105.91 -94.00 -30.00  130
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0874137000
_diffrn_orient_matrix_UB_12      0.0541032000
_diffrn_orient_matrix_UB_13      -0.0322564000
_diffrn_orient_matrix_UB_21      -0.0101322000
_diffrn_orient_matrix_UB_22      -0.1434015000
_diffrn_orient_matrix_UB_23      -0.0383013000
_diffrn_orient_matrix_UB_31      -0.0820466000
_diffrn_orient_matrix_UB_32      0.0752911000
_diffrn_orient_matrix_UB_33      -0.0497567000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31399
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.821
_diffrn_reflns_theta_min         3.648
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.271
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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_density_diffrn    1.379
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.647
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5290
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0749P)^2^+0.7568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4878
_reflns_number_total             5290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06975k2.cif
_cod_data_source_block           PD-673_auto_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7135428
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.715
_shelx_estimated_absorpt_t_max   0.828
_cell_oxdiff_length_a            13.0535(2)
_cell_oxdiff_length_b            9.02166(16)
_cell_oxdiff_length_c            22.2478(3)
_cell_oxdiff_angle_alpha         90.0023(13)
_cell_oxdiff_angle_beta          101.2077(12)
_cell_oxdiff_angle_gamma         90.0131(14)
_cell_oxdiff_volume              2570.02(7)
_cell_oxdiff_measurement_reflns_used 18949
_oxdiff_exptl_absorpt_empirical_full_min 0.605
_oxdiff_exptl_absorpt_empirical_full_max 2.000
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01b1d7d5f3778207ef9c1304a01e600ae003576931a
;
_diffrn_oxdiff_digest_hkl
;
014c55771fdcc386736b83f1a12cc5d3e9937b
;
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C28 H25 P2 S2 N1 O2'
_chemical_oxdiff_usercomment     'vapor diffusion thf-hex'
_shelx_res_checksum              41608