Covalent capture of nitrous oxide by phosphanides.
Genoux, Alexandre; Wong, Tak Hin; Fadaei-Tirani, Farzaneh; Severin, Kay; Chemical communications (Cambridge, England) 61 (2025) 15654–15657; doi:10.1039/d5cc04154f

data_7134979
_publ_section_title
;
 Covalent capture of nitrous oxide by phosphanides.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15654
_journal_page_last               15657
_journal_paper_doi               10.1039/d5cc04154f
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C18 H36 K N2 O6, C8 H18 N2 O P'
_chemical_formula_sum            'C26 H54 K N4 O7 P'
_chemical_formula_weight         604.80
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-06-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-07-17 deposited with the CCDC.	2025-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.469(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2179(6)
_cell_length_b                   8.7318(2)
_cell_length_c                   21.9955(7)
_cell_measurement_reflns_used    3620
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      71.9130
_cell_measurement_theta_min      4.0950
_cell_volume                     3215.92(18)
_computing_cell_refinement       'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 44.111a 64-bit (release 13-05-2025))'
_computing_data_reduction        'CrysAlisPro 1.171.44.111a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_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    -38.00  34.00   1.00   10.00    --  -40.66  31.00 -28.00   72
  2  \w    -87.00 -13.00   1.00   10.00    --  -40.66 -31.00 171.00   74
  3  \w     -8.00  17.00   1.00   10.00    --   40.66 -31.00 171.00   25
  4  \w     41.00  66.00   1.00   10.00    --   40.66  31.00 -28.00   25
  5  \w    101.00 177.00   1.00   50.00    --  105.15  31.00 -28.00   76
  6  \w     30.00 113.00   1.00   50.00    --  105.15 -31.00 171.00   83
  7  \w     52.00  82.00   1.00   10.00    --   40.66-125.00 -90.00   30
  8  \w     44.00  97.00   1.00   10.00    --   40.66-125.00  30.00   53
  9  \w     18.00 104.00   1.00   10.00    --   40.66  38.00-180.00   86
 10  \w    104.00 178.00   1.00   50.00    --  105.15  77.00 -90.00   74
 11  \w     66.00 118.00   1.00   50.00    --  105.15 -45.00  90.00   52
 12  \w    107.00 134.00   1.00   50.00    --  105.15 111.00-150.00   27
 13  \w    103.00 141.00   1.00   50.00    --  105.15 178.00-180.00   38
 14  \w     65.00  93.00   1.00   50.00    --  105.15 178.00-180.00   28
 15  \w     32.00 104.00   1.00   50.00    --  105.15 -94.00-150.00   72
 16  \w    131.00 156.00   1.00   50.00    --  105.15 111.00-180.00   25
 17  \w     33.00  97.00   1.00   50.00    --  105.15 -94.00 120.00   64
;
_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      0.0048334000
_diffrn_orient_matrix_UB_12      -0.0220261000
_diffrn_orient_matrix_UB_13      0.0702834000
_diffrn_orient_matrix_UB_21      -0.0850449000
_diffrn_orient_matrix_UB_22      -0.0674339000
_diffrn_orient_matrix_UB_23      -0.0154019000
_diffrn_orient_matrix_UB_31      0.0346864000
_diffrn_orient_matrix_UB_32      -0.1615690000
_diffrn_orient_matrix_UB_33      -0.0032044000
_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  0.0742
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.735
_diffrn_reflns_theta_min         4.133
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.298
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.111a (Rigaku Oxford Diffraction, 2025)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0945P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1543
_refine_ls_wR_factor_ref         0.1752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4338
_reflns_number_total             6239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04154f2.cif
_cod_data_source_block           ga-306
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7134977--7134981.cif.
;
_cod_original_cell_volume        3215.94(18)
_cod_database_code               7134979
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C26 H54 K N4 O7 P'
_chemical_oxdiff_usercomment     'THF, HEXANE, CRYPTAND'
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.754
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B),
  C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              36660
_shelx_hkl_checksum              65636
_olex2_date_sample_data_collection 2025-05-22
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 2.235
_oxdiff_exptl_absorpt_empirical_full_min 0.457