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_7135429
_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         'C104 H106 K6 N2 O11 P6 Se6, 3(C4 H8 O)'
_chemical_formula_sum            'C116 H130 K6 N2 O14 P6 Se6'
_chemical_formula_weight         2670.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-05
_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                 113.1020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.5782(2)
_cell_length_b                   14.67560(10)
_cell_length_c                   31.7159(2)
_cell_measurement_reflns_used    71807
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      76.3740
_cell_measurement_theta_min      2.8240
_cell_volume                     11806.90(16)
_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 (G.M. Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110(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   -118.00 -54.00   0.50    1.60    --  -47.28-153.00  -0.00  128
  2  \w    -72.00 -46.00   0.50    1.60    --  -47.28 121.00-118.00   52
  3  \w   -103.00 -76.00   0.50    1.60    --  -47.28 153.00  39.00   54
  4  \w     44.00  92.00   0.50    1.60    --   47.28-121.00 157.00   96
  5  \w     50.00  91.00   0.50    1.60    --   47.28-153.00  -0.00   82
  6  \w   -144.00-119.00   0.50    7.20    --  -91.75-121.00 157.00   50
  7  \w    -90.00 -65.00   0.50    7.20    --  -91.75 153.00  39.00   50
  8  \w   -137.00 -93.00   0.50    7.20    --  -91.75-153.00  -0.00   88
  9  \w    -75.00 -25.00   0.50    7.20    --  -91.75 121.00-118.00  100
 10  \w     69.00 108.00   0.50    7.20    --  105.91-121.00 157.00   78
 11  \w     82.00 135.00   0.50    7.20    --  105.91 153.00  39.00  106
 12  \w     98.00 164.00   0.50    7.20    --  105.91 121.00-118.00  132
 13  \w     57.00 130.00   0.50    7.20    --  105.91-153.00  -0.00  146
 14  \w    -18.00  18.00   0.50    1.60    --  -47.28  19.00-120.00   72
 15  \w    -11.00  14.00   0.50    1.60    --  -47.28  19.00 -90.00   50
 16  \w    -23.00  25.00   0.50    1.60    --  -47.28  19.00 -30.00   96
 17  \w     -7.00  18.00   0.50    1.60    --  -47.28  19.00 150.00   50
 18  \w   -117.00 -26.00   0.50    1.60    --  -47.28 -77.00   0.00  182
 19  \w     33.00 116.00   0.50    1.60    --   47.28  57.00  90.00  166
 20  \w   -162.00 -77.00   0.50    7.20    --  -91.75 -61.00-180.00  170
 21  \w   -164.00 -89.00   0.50    7.20    --  -91.75 -15.00  30.00  150
 22  \w   -163.00-105.00   0.50    7.20    --  -91.75 -45.00-150.00  116
 23  \w    -45.00 -20.00   0.50    7.20    --  -91.75  45.00 120.00   50
 24  \w   -131.00 -80.00   0.50    7.20    --  -91.75 -30.00-150.00  102
 25  \w    -45.00 -20.00   0.50    7.20    --  -91.75  45.00  30.00   50
 26  \w     33.00  73.00   0.50    7.20    --  105.91 -61.00 120.00   80
 27  \w     79.00 105.00   0.50    7.20    --  105.91 -94.00-150.00   52
 28  \w     53.00 112.00   0.50    7.20    --  105.91-125.00 120.00  118
 29  \w     44.00 111.00   0.50    7.20    --  105.91-125.00-150.00  134
 30  \w    137.00 177.00   0.50    7.20    --  105.91  45.00-120.00   80
 31  \w     46.00 105.00   0.50    7.20    --  105.91 -95.00-173.31  118
 32  \w     95.00 131.00   0.50    7.20    --  105.91  45.00-120.00   72
 33  \w     33.00  62.00   0.50    7.20    --  105.91 -61.00 -60.00   58
 34  \w     85.00 112.00   0.50    7.20    --  105.91-125.00  60.00   54
 35  \w     36.00 108.00   0.50    7.20    --  105.91 -77.00-180.00  144
 36  \w     33.00  77.00   0.50    7.20    --  105.91 -94.00   0.00   88
 37  \w     49.00  75.00   0.50    7.20    --  105.91-125.00  60.00   52
 38  \w    127.00 154.00   0.50    7.20    --  105.91 125.00-180.00   54
 39  \w     83.00 172.00   0.50    7.20    --  105.91  77.00  30.00  178
 40  \w     61.00 106.00   0.50    7.20    --  105.91 -94.00 -30.00   90
 41  \w     33.00  73.00   0.50    7.20    --  105.91 -94.00  30.00   80
 42  \w     79.00 105.00   0.50    7.20    --  105.91 -94.00  30.00   52
 43  \w     86.00 158.00   0.50    7.20    --  105.91  77.00 -60.00  144
;
_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      0.0028656000
_diffrn_orient_matrix_UB_12      0.0065332000
_diffrn_orient_matrix_UB_13      0.0493993000
_diffrn_orient_matrix_UB_21      0.0534896000
_diffrn_orient_matrix_UB_22      -0.0496825000
_diffrn_orient_matrix_UB_23      0.0176663000
_diffrn_orient_matrix_UB_31      0.0286195000
_diffrn_orient_matrix_UB_32      0.0922474000
_diffrn_orient_matrix_UB_33      0.0060027000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            159656
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.999
_diffrn_reflns_theta_min         2.841
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.346
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.558
_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    1.502
_exptl_crystal_description       plate
_exptl_crystal_F_000             5440
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1535
_refine_ls_number_reflns         21491
_refine_ls_number_restraints     762
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0328P)^2^+63.0244P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19443
_reflns_number_total             21491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc06975k2.cif
_cod_data_source_block           PD-416_auto_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7135429
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.501
_shelx_estimated_absorpt_t_max   0.674
_cell_oxdiff_length_a            27.5775(2)
_cell_oxdiff_length_b            14.67494(13)
_cell_oxdiff_length_c            31.7173(3)
_cell_oxdiff_angle_alpha         89.9819(7)
_cell_oxdiff_angle_beta          113.0987(9)
_cell_oxdiff_angle_gamma         90.0164(7)
_cell_oxdiff_volume              11806.86(18)
_cell_oxdiff_measurement_reflns_used 71803
_oxdiff_exptl_absorpt_empirical_full_min 0.530
_oxdiff_exptl_absorpt_empirical_full_max 3.088
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01b373aaa7071d7fce3e47f04d29a5601c040647f43
;
_diffrn_oxdiff_digest_hkl
;
01336ed76ef34d568264c21555ab81966e84c6
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_theta     66.97
_reflns_odcompleteness_iscentric 1
_chemical_oxdiff_formula         'c116 H129 N2 O14 P6 K6 Se6'
_chemical_oxdiff_usercomment     'conc solution in thf-d8 at rt'
_shelx_res_checksum              58265