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_7135430
_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         'C108 H114 K6 N2 O12 P6 S6'
_chemical_formula_sum            'C108 H114 K6 N2 O12 P6 S6'
_chemical_formula_weight         2244.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2025-11-21
_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                 98.1107(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.33755(12)
_cell_length_b                   22.84495(10)
_cell_length_c                   23.04768(11)
_cell_measurement_reflns_used    133955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.5000
_cell_measurement_theta_min      2.6240
_cell_volume                     12686.11(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS (G.M. Sheldrick, 1997)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -22.00   3.00   0.50    1.50    --  -47.03  19.00 114.00   50
  2  \w     37.00  71.00   0.50    1.50    --   47.03  19.00 114.00   68
  3  \w     78.00 103.00   0.50    1.50    --   47.03  19.00 114.00   50
  4  \w    -25.00  29.00   0.50    1.50    --   47.03 -19.00 -53.00  108
  5  \w   -135.00 -91.00   0.50    6.00    --  -91.75 -19.00 -53.00   88
  6  \w     93.00 153.00   0.50    6.00    --  105.91  19.00 114.00  120
  7  \w    -43.00 -17.00   0.50    1.50    --    6.00 127.00-148.52   52
  8  \w    -60.00 -35.00   0.50    1.50    --   14.00 166.00 -80.39   50
  9  \w    -12.00  14.00   0.50    1.50    --   18.00  98.00 109.09   52
 10  \w     -7.00  18.00   0.50    1.50    --   26.00  99.00 -22.80   50
 11  \w      1.00  26.00   0.50    1.50    --   34.00  98.00 122.78   50
 12  \w      7.00  32.00   0.50    1.50    --   38.00  94.00 -70.63   50
 13  \w     13.00  38.00   0.50    1.50    --   42.00  91.00  63.68   50
 14  \w     17.00  42.00   0.50    1.50    --   46.00  90.00 -16.33   50
 15  \w     17.00  42.00   0.50    1.50    --   46.00  90.00-122.27   50
 16  \w     17.00  42.00   0.50    1.50    --   46.00  90.00-145.06   50
 17  \w   -104.00 -57.00   0.50    1.50    --  -47.03 -19.00 -53.00   94
 18  \w    -69.00 -39.00   0.50    1.50    --  -47.03 -19.00  60.00   60
 19  \w    -85.00 -22.00   0.50    1.50    --  -47.03 125.00 150.00  126
 20  \w   -102.00 -74.00   0.50    1.50    --  -47.03 -19.00  60.00   56
 21  \w    -98.00 -36.00   0.50    1.50    --  -47.03 -19.00-150.00  124
 22  \w     36.00  93.00   0.50    1.50    --   47.03-125.00 150.00  114
 23  \w     53.00  84.00   0.50    1.50    --   47.03-125.00-150.00   62
 24  \w     90.00 116.00   0.50    1.50    --   50.00  77.00 168.59   52
 25  \w     27.00  59.00   0.50    1.50    --   50.00  77.00 168.59   64
 26  \w     29.00  75.00   0.50    1.50    --   50.00  75.00-167.33   92
 27  \w     32.00  64.00   0.50    1.50    --   54.00  75.00 123.07   64
 28  \w     37.00  63.00   0.50    1.50    --   58.00  76.00-140.43   52
 29  \w     75.00 108.00   0.50    1.50    --   58.00  75.00  82.50   66
 30  \w     35.00  81.00   0.50    1.50    --   58.00  77.00 -75.71   92
 31  \w     38.00  70.00   0.50    1.50    --   58.00  73.00 -12.49   64
 32  \w     35.00  60.00   0.50    1.50    --   58.00  77.00  57.36   50
 33  \w     35.00  61.00   0.50    1.50    --   58.00  77.00-178.74   52
 34  \w     36.00  66.00   0.50    1.50    --   58.00  75.00  82.50   60
 35  \w     37.00  63.00   0.50    1.50    --   58.00  74.00-101.42   52
 36  \w     93.00 120.00   0.50    1.50    --   62.00  75.00 -46.11   54
 37  \w     41.00  86.00   0.50    1.50    --   62.00  75.00 -46.11   90
 38  \w     40.00  65.00   0.50    1.50    --   62.00  76.00 156.28   50
 39  \w     39.00  64.00   0.50    1.50    --   62.00  77.00  27.29   50
 40  \w    -81.00 -47.00   0.50    1.50    --  -66.00 -69.00 -47.47   68
 41  \w    -80.00 -48.00   0.50    1.50    --  -66.00 -70.00 -20.56   64
 42  \w     47.00  73.00   0.50    1.50    --   70.00  77.00-157.80   52
 43  \w     48.00  79.00   0.50    1.50    --   70.00  77.00  95.90   62
 44  \w    119.00 144.00   0.50    1.50    --   74.00  77.00  69.30   50
 45  \w     52.00  78.00   0.50    1.50    --   74.00  77.00  69.30   52
 46  \w    -81.00 -52.00   0.50    6.00    --  -74.00 -75.00 159.89   58
 47  \w    -81.00 -53.00   0.50    6.00    --  -74.00 -72.00  27.81   56
 48  \w    -87.00 -57.00   0.50    6.00    --  -74.00 -65.00-134.73   60
 49  \w    -83.00 -57.00   0.50    6.00    --  -78.00 -74.00-141.08   52
 50  \w    -90.00 -59.00   0.50    6.00    --  -78.00 -73.00 172.37   62
 51  \w    -83.00 -57.00   0.50    6.00    --  -78.00 -72.00 -94.15   52
 52  \w    -82.00 -56.00   0.50    6.00    --  -78.00 -75.00 129.93   52
 53  \w    -82.00 -56.00   0.50    6.00    --  -78.00 -74.00  20.11   52
 54  \w    -90.00 -56.00   0.50    6.00    --  -78.00 -74.00 145.38   68
 55  \w    -96.00 -55.00   0.50    6.00    --  -78.00 -77.00 116.60   82
 56  \w    -84.00 -58.00   0.50    6.00    --  -78.00 -71.00 -17.14   52
 57  \w    -81.00 -56.00   0.50    6.00    --  -78.00 -75.00-123.61   50
 58  \w    -89.00 -61.00   0.50    6.00    --  -82.00 -72.00 -30.23   56
 59  \w    -87.00 -61.00   0.50    6.00    --  -82.00 -73.00-155.09   52
 60  \w   -145.00-119.00   0.50    6.00    --  -86.00 -74.00  89.13   52
 61  \w    -89.00 -63.00   0.50    6.00    --  -86.00 -76.00  64.94   52
 62  \w    -96.00 -64.00   0.50    6.00    --  -86.00 -75.00 -53.56   64
 63  \w    -91.00 -65.00   0.50    6.00    --  -86.00 -74.00  89.13   52
 64  \w   -160.00 -67.00   0.50    6.00    --  -90.00 -76.00 129.99  186
 65  \w   -161.00 -68.00   0.50    6.00    --  -90.00 -75.00-106.11  186
 66  \w   -162.00-131.00   0.50    6.00    --  -91.75 -77.00 -90.00   62
 67  \w   -144.00 -72.00   0.50    6.00    --  -91.75 -75.00 160.93  144
 68  \w   -135.00 -72.00   0.50    6.00    --  -91.75 -75.00 -26.18  126
 69  \w   -134.00 -70.00   0.50    6.00    --  -91.75 -77.00 120.00  128
 70  \w   -158.00 -74.00   0.50    6.00    --  -91.75 -74.00  67.21  168
 71  \w    -47.00 -20.00   0.50    6.00    --  -91.75  45.00-180.00   54
 72  \w   -150.00 -71.00   0.50    6.00    --  -91.75 -71.00 -44.41  158
 73  \w    -55.00 -28.00   0.50    6.00    --  -91.75  77.00-120.00   54
 74  \w   -142.00 -69.00   0.50    6.00    --  -91.75 -77.00  60.00  146
 75  \w    -98.00 -72.00   0.50    6.00    --  -91.75 -71.00  25.98   52
 76  \w    -96.00 -69.00   0.50    6.00    --  -91.75 -77.00-180.00   54
 77  \w   -155.00-110.00   0.50    6.00    --  -91.75 -77.00-180.00   90
 78  \w   -156.00 -72.00   0.50    6.00    --  -91.75 -75.00 -75.98  168
 79  \w    -99.00 -74.00   0.50    6.00    --  -91.75 -74.00  44.28   50
 80  \w    -94.00 -69.00   0.50    6.00    --  -91.75 -77.00  91.65   50
 81  \w    -68.00 -19.00   0.50    6.00    --  -91.75  61.00 -30.00   98
 82  \w   -106.00 -69.00   0.50    6.00    --  -91.75 -77.00-120.00   74
 83  \w   -143.00 -70.00   0.50    6.00    --  -91.75 -77.00 -60.00  146
 84  \w   -116.00 -72.00   0.50    6.00    --  -91.75 -71.00-141.97   88
 85  \w   -158.00-121.00   0.50    6.00    --  -91.75 -74.00  44.28   74
 86  \w    -47.00 -20.00   0.50    6.00    --  -91.75  45.00  30.00   54
 87  \w    -47.00 -21.00   0.50    6.00    --  -91.75  45.00 -90.00   52
 88  \w   -146.00-120.00   0.50    6.00    --  -91.75 -71.00-141.97   52
 89  \w   -163.00 -71.00   0.50    6.00    --  -91.75 -77.00-150.00  184
 90  \w    -84.00 -30.00   0.50    6.00    --  -91.75 125.00  60.00  108
 91  \w   -155.00 -71.00   0.50    6.00    --  -91.75 -71.00  14.85  168
 92  \w    -99.00 -70.00   0.50    6.00    --  -91.75  77.00-120.00   58
 93  \w    -97.00 -72.00   0.50    6.00    --  -91.75 -69.00 -19.32   50
 94  \w   -141.00 -71.00   0.50    6.00    --  -91.75 -72.00-170.94  140
 95  \w   -141.00-116.00   0.50    6.00    --  -91.75 -71.00   4.69   50
 96  \w   -101.00 -71.00   0.50    6.00    --  -91.75 -71.00   4.69   60
 97  \w   -159.00-133.00   0.50    6.00    --  -91.75 -69.00 -19.32   52
 98  \w    -94.00 -69.00   0.50    6.00    --  -91.75 -77.00 -90.00   50
 99  \w     36.00  73.00   0.50    6.00    --  105.91 -61.00-180.00   74
100  \w     38.00 111.00   0.50    6.00    --  105.91-125.00-180.00  146
101  \w     37.00 110.00   0.50    6.00    --  105.91-125.00 -60.00  146
102  \w     72.00 124.00   0.50    6.00    --  105.91-141.00  49.51  104
103  \w     82.00 112.00   0.50    6.00    --  105.91-125.00 -90.00   60
104  \w     36.00  74.00   0.50    6.00    --  105.91-125.00 -90.00   76
105  \w     81.00 111.00   0.50    6.00    --  105.91-125.00  90.00   60
106  \w     42.00  69.00   0.50    6.00    --  105.91 -61.00 150.00   54
107  \w     41.00  66.00   0.50    6.00    --  105.91-125.00  90.00   50
108  \w     34.00 106.00   0.50    6.00    --  105.91 -77.00   0.00  144
109  \w     42.00 103.00   0.50    6.00    --  105.91 -94.00 -30.00  122
110  \w     80.00 111.00   0.50    6.00    --  105.91-125.00 150.00   62
111  \w     46.00  72.00   0.50    6.00    --  105.91-125.00 150.00   52
112  \w     48.00  73.00   0.50    6.00    --  105.91 -61.00  30.00   50
113  \w     82.00 107.00   0.50    6.00    --  105.91-131.00 -18.55   50
114  \w     38.00  70.00   0.50    6.00    --  105.91-131.00 -18.55   64
;
_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      -0.0140269000
_diffrn_orient_matrix_UB_12      -0.0437325000
_diffrn_orient_matrix_UB_13      -0.0508633000
_diffrn_orient_matrix_UB_21      -0.0079865000
_diffrn_orient_matrix_UB_22      0.0512208000
_diffrn_orient_matrix_UB_23      -0.0437851000
_diffrn_orient_matrix_UB_31      0.0618765000
_diffrn_orient_matrix_UB_32      -0.0032545000
_diffrn_orient_matrix_UB_33      -0.0073494000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            189911
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         2.665
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.175
_exptl_crystal_description       plate
_exptl_crystal_F_000             4688
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.022(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1354
_refine_ls_number_reflns         22119
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0625P)^2^+22.0554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.955
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                21830
_reflns_number_total             22119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06975k2.cif
_cod_data_source_block           PD-681_full_sq
_cod_original_cell_volume        12686.10(10)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7135430
_shelx_shelxl_version_number     2019/3
_cell_oxdiff_length_a            24.33403(14)
_cell_oxdiff_length_b            22.84715(10)
_cell_oxdiff_length_c            23.04829(10)
_cell_oxdiff_angle_alpha         90.0657(4)
_cell_oxdiff_angle_beta          98.1017(4)
_cell_oxdiff_angle_gamma         90.0296(4)
_cell_oxdiff_volume              12686.10(11)
_cell_oxdiff_measurement_reflns_used 133956
_oxdiff_exptl_absorpt_empirical_full_min 0.776
_oxdiff_exptl_absorpt_empirical_full_max 1.499
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'C121 H127 N2 O14 P6 S6 K6'
_chemical_oxdiff_usercomment     'vapor diffusion thf-hex'
_shelx_res_checksum              61185
_shelx_fab_checksum              70017