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_7134978
_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, C20 H30 N2 O P, 2[C4H8O]'
_chemical_formula_sum            'C46 H82 K N4 O9 P'
_chemical_formula_weight         905.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-06-04
_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                 95.713(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2324(5)
_cell_length_b                   11.8181(6)
_cell_length_c                   36.8937(13)
_cell_measurement_reflns_used    8153
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      66.2410
_cell_measurement_theta_min      2.3780
_cell_volume                     4873.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.135a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.134a 64-bit (release 09-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.135a (Rigaku OD, 2024)'
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     28.00  53.00   0.50    6.00    --   66.04-100.00 -56.00   50
  2  \w    -77.00 -52.00   0.50    6.00    --  -66.76 100.00  48.00   50
  3  \w    -62.00 -36.00   0.50    6.00    --  -69.34 100.00  48.00   52
  4  \w     32.00  80.00   0.50    6.00    --   69.57-100.00 -56.00   96
  5  \w     42.00  68.00   0.50    6.00    --   77.93-100.00 -56.00   52
  6  \w     33.00  71.00   0.50    6.00    --   66.04 -95.00 150.00   76
  7  \w     29.00  73.00   0.50    6.00    --   66.04 -95.00 -90.00   88
  8  \w     30.00  59.00   0.50    6.00    --   66.04 -95.00   0.00   58
  9  \w     30.00  70.00   0.50    6.00    --   66.04 -95.00  90.00   80
 10  \w   -111.00 -83.00   0.50    6.00    --  -66.76 -15.00  60.00   56
 11  \w    -69.00 -30.00   0.50    6.00    --  -66.76   0.00 150.00   78
 12  \w    -66.00 -38.00   0.50    6.00    --  -66.76 -15.00  60.00   56
 13  \w    -71.00 -29.00   0.50    6.00    --  -66.76   0.00  60.00   84
 14  \w   -113.00 -51.00   0.50    6.00    --  -69.34 -15.00 150.00  124
 15  \w    -68.00 -40.00   0.50    6.00    --  -69.34   0.00-180.00   56
 16  \w    -69.00 -38.00   0.50    6.00    --  -69.34   0.00  30.00   62
 17  \w    -94.00 -37.00   0.50    6.00    --  -69.34 125.00 -60.00  114
 18  \w     37.00  78.00   0.50    6.00    --   69.57 -95.00-180.00   82
 19  \w     33.00  93.00   0.50    6.00    --   69.57-125.00 120.00  120
 20  \w     45.00 108.00   0.50    6.00    --   77.93   0.00 120.00  126
 21  \w     68.00 101.00   0.50    6.00    --   77.93-125.00   0.00   66
 22  \w     40.00  66.00   0.50    6.00    --   77.93 -95.00-150.00   52
 23  \w     42.00 104.00   0.50    6.00    --   77.93-125.00 150.00  124
 24  \w     51.00  98.00   0.50    6.00    --   77.93  15.00  30.00   94
 25  \w     67.00 103.00   0.50    6.00    --   77.93   0.00-120.00   72
 26  \w     76.00 101.00   0.50    6.00    --   77.93-125.00  30.00   50
 27  \w     41.00  84.00   0.50    6.00    --   77.93 -95.00-120.00   86
 28  \w     46.00  71.00   0.50    6.00    --   77.93 -95.00 120.00   50
 29  \w     47.00 100.00   0.50    6.00    --   77.93-125.00  60.00  106
 30  \w     70.00 108.00   0.50    6.00    --   77.93  15.00 -60.00   76
 31  \w     59.00  84.00   0.50    6.00    --   77.93 -95.00  30.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0083398000
_diffrn_orient_matrix_UB_12      0.1233227000
_diffrn_orient_matrix_UB_13      0.0134801000
_diffrn_orient_matrix_UB_21      -0.1280112000
_diffrn_orient_matrix_UB_22      -0.0084906000
_diffrn_orient_matrix_UB_23      0.0114472000
_diffrn_orient_matrix_UB_31      0.0508838000
_diffrn_orient_matrix_UB_32      -0.0410349000
_diffrn_orient_matrix_UB_33      0.0380457000
_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  0.1184
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            31097
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        50.429
_diffrn_reflns_theta_max         50.429
_diffrn_reflns_theta_min         2.407
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.715
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.135a (Rigaku Oxford Diffraction, 2024)
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    1.234
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     861
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0997
_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^)+(0.1953P)^2^+2.9985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2896
_refine_ls_wR_factor_ref         0.3123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3243
_reflns_number_total             5095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04154f2.cif
_cod_data_source_block           ga-194-1
_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        4873.1(4)
_cod_database_code               7134978
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C46 H82 K N4 O9 P'
_chemical_oxdiff_usercomment     'crystallised from THF'
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C13(H13), C15(H15), C17(H17)
4.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
  C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C2(H2A,H2B),
 C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C12(H12A,
 H12B), C14(H14A,H14B), C16(H16A,H16B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 294 electrons were 
found in a volume of 1218\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2[C4H8O] per Asymmetric Unit 
which account for 320 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              67916
_shelx_hkl_checksum              67376
_shelx_fab_checksum              43320
_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 8.870
_oxdiff_exptl_absorpt_empirical_full_min 0.173