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_7134980
_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         'C47 H66 Au N2 O P, 2.5[C4H8O]'
_chemical_formula_sum            'C57 H86 Au N2 O3.5 P'
_chemical_formula_weight         1083.21
_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                 114.7071(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.92474(18)
_cell_length_b                   22.02986(18)
_cell_length_c                   15.23246(18)
_cell_measurement_reflns_used    24178
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.6800
_cell_measurement_theta_min      2.7030
_cell_volume                     5464.35(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.135a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.137a 64-bit (release 10-09-2024))'
_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 0.999
_diffrn_measured_fraction_theta_max 0.961
_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     49.00 119.00   0.50    0.30    --   77.93  15.00 -60.00  140
  2  \w     79.00 106.00   0.50    0.30    --   69.57   0.00 -30.00   54
  3  \w     37.00  74.00   0.50    0.30    --   69.57   0.00 -30.00   74
  4  \w     42.00  87.00   0.50    0.30    --   69.57  15.00  30.00   90
  5  \w     42.00  98.00   0.50    0.30    --   77.93   0.00  30.00  112
  6  \w     30.00  72.00   0.50    0.30    --   66.04 -95.00  90.00   84
  7  \w     54.00  94.00   0.50    0.30    --   69.57-125.00 150.00   80
  8  \w     36.00 100.00   0.50    0.30    --   77.93-125.00  60.00  128
  9  \w     75.00 100.00   0.50    0.30    --   77.93-125.00  30.00   50
 10  \w     37.00  62.00   0.50    0.30    --   77.93-125.00  30.00   50
 11  \w     40.00  73.00   0.50    0.30    --   77.93 -95.00 150.00   66
 12  \w     55.00  85.00   0.50    0.30    --   77.93 -95.00  60.00   60
 13  \w     60.00  85.00   0.50    0.30    --   77.93 -95.00  90.00   50
 14  \w     41.00  71.00   0.50    0.30    --   66.04 -95.00  30.00   60
 15  \w     43.00  68.00   0.50    0.30    --   77.93 -95.00 120.00   50
 16  \w     32.00  76.00   0.50    0.30    --   69.57 -95.00   0.00   88
 17  \w     28.00  75.00   0.50    0.30    --   66.04 -95.00 -60.00   94
 18  \w     48.00  86.00   0.50    0.30    --   77.93 -95.00-150.00   76
 19  \w     42.00  77.00   0.50    0.30    --   69.57 -95.00-180.00   70
 20  \w    -65.00 -39.00   0.50    0.30    --  -66.76   0.00  30.00   52
 21  \w    -58.00 -30.00   0.50    0.30    --  -66.76   0.00  60.00   56
 22  \w    -62.00 -32.00   0.50    0.30    --  -69.34   0.00 -90.00   60
 23  \w    -58.00 -32.00   0.50    0.30    --  -69.34   0.00 -30.00   52
 24  \w    -60.00 -35.00   0.50    0.30    --  -66.76 -15.00   0.00   50
 25  \w   -111.00 -73.00   0.50    0.30    --  -66.76 -15.00   0.00   76
 26  \w    -64.00 -27.00   0.50    0.30    --  -66.76 125.00  30.00   74
 27  \w    -83.00 -27.00   0.50    0.30    --  -69.34 125.00 120.00  112
;
_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      0.0169855000
_diffrn_orient_matrix_UB_12      -0.0106310000
_diffrn_orient_matrix_UB_13      -0.0899772000
_diffrn_orient_matrix_UB_21      -0.0398278000
_diffrn_orient_matrix_UB_22      -0.0632780000
_diffrn_orient_matrix_UB_23      -0.0131143000
_diffrn_orient_matrix_UB_31      -0.0840852000
_diffrn_orient_matrix_UB_32      0.0277817000
_diffrn_orient_matrix_UB_33      -0.0643047000
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47812
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.679
_diffrn_reflns_theta_min         3.375
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.664
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.534
_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    1.317
_exptl_crystal_description       plate
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.008
_refine_diff_density_max         1.152
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.000143(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         10776
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9137
_reflns_number_total             10776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04154f2.cif
_cod_data_source_block           ga-210
_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_formula_sum        'C57 H86 Au N2 O3.50 P'
_cod_database_code               7134980
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C57 H86 Au N2 O3.50 P'
_chemical_oxdiff_usercomment     'CRYSTALLISED FROM THF'
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.484
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C10 \\sim C11 \\sim C12: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
3.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C30(H30), C33(H33), C34(H34),
 C40(H40), C42(H42), C44(H44)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B),
 C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 433 electrons were 
found in a volume of 1773\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.5[C4H8O] per Asymmetric Unit 
which account for 400 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              19111
_shelx_hkl_checksum              80538
_shelx_fab_checksum              51345
_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 1.618
_oxdiff_exptl_absorpt_empirical_full_min 0.700