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_7134977
_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         'C60 H90 Cl4 Ir2 Li2 O2 P2, C4 H8 O'
_chemical_formula_sum            'C64 H98 Cl4 Ir2 Li2 O3 P2'
_chemical_formula_weight         1517.44
_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             2025-06-04
_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                 99.0460(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.52239(8)
_cell_length_b                   18.32736(16)
_cell_length_c                   17.04898(11)
_cell_measurement_reflns_used    29587
_cell_measurement_temperature    139.99(10)
_cell_measurement_theta_max      74.5010
_cell_measurement_theta_min      3.5520
_cell_volume                     3246.96(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.130a 64-bit (release 05-07-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (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      139.99(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 0.998
_diffrn_measured_fraction_theta_max 0.977
_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    -99.00 -74.00   0.50    0.10    --  -71.12 153.00-165.00   50
  2  \w   -108.00 -82.00   0.50    0.10    --  -64.59 153.00-165.00   52
  3  \w   -113.00 -79.00   0.50    0.10    --  -76.25 139.00 -31.14   68
  4  \w   -107.00 -79.00   0.50    0.10    --  -76.25 130.00 -33.19   56
  5  \w    -73.00 -47.00   0.50    0.10    --  -76.25 125.00 -37.21   52
  6  \w   -101.00 -75.00   0.50    0.10    --  -76.25 125.00 -37.21   52
  7  \w   -107.00 -71.00   0.50    0.10    --  -76.25 130.00  13.32   72
  8  \w    -80.00 -55.00   0.50    0.10    --  -64.59 122.00  34.00   50
  9  \w    -76.00 -34.00   0.50    0.10    --  -71.12 122.00  34.00   84
 10  \w    -67.00 -38.00   0.50    0.10    --  -71.12   0.00 120.00   58
 11  \w    -70.00 -34.00   0.50    0.10    --  -71.12   0.00  30.00   72
 12  \w    -69.00 -34.00   0.50    0.10    --  -71.12   0.00 -90.00   70
 13  \w   -113.00 -88.00   0.50    0.10    --  -76.25 -73.00 -25.42   50
 14  \w   -111.00 -86.00   0.50    0.10    --  -76.25 -77.00  -9.04   50
 15  \w   -110.00 -85.00   0.50    0.10    --  -76.25 -74.00  54.01   50
 16  \w   -111.00 -82.00   0.50    0.10    --  -76.25 -75.00 114.81   58
 17  \w   -102.00 -77.00   0.50    0.10    --  -64.59-153.00 153.00   50
 18  \w   -107.00 -56.00   0.50    0.10    --  -71.12-153.00 153.00  102
 19  \w     47.00  72.00   0.50    0.10    --   63.87-153.00 153.00   50
 20  \w     55.00  80.00   0.50    0.10    --   75.73-153.00 153.00   50
 21  \w     56.00  81.00   0.50    0.10    --   76.61-153.00 153.00   50
 22  \w     87.00 116.00   0.50    0.10    --   79.75-138.00 -39.07   58
 23  \w     46.00  75.00   0.50    0.10    --   79.75-138.00 -39.07   58
 24  \w     36.00  61.00   0.50    0.10    --   76.61-125.00   0.00   50
 25  \w     65.00 100.00   0.50    0.10    --   76.61-125.00  90.00   70
 26  \w     59.00 101.00   0.50    0.10    --   76.61-125.00 120.00   84
 27  \w     75.00 101.00   0.50    0.10    --   76.61-125.00   0.00   52
 28  \w     68.00  93.00   0.50    0.10    --   76.61-122.00 -47.00   50
 29  \w     31.00  56.00   0.50    0.10    --   63.87-122.00 -47.00   50
 30  \w     46.00  99.00   0.50    0.10    --   79.75-113.00  10.38  106
 31  \w     37.00  71.00   0.50    0.10    --   75.73-111.00 -90.00   68
 32  \w     28.00  64.00   0.50    0.10    --   63.87 -95.00-120.00   72
 33  \w     43.00  68.00   0.50    0.10    --   76.61 -95.00 -90.00   50
 34  \w     52.00  77.00   0.50    0.10    --   76.61 -95.00-120.00   50
 35  \w     55.00  80.00   0.50    0.10    --   76.61 -95.00-180.00   50
 36  \w     41.00  67.00   0.50    0.10    --   76.61 -95.00  60.00   52
 37  \w     45.00  74.00   0.50    0.10    --   76.61 -95.00 150.00   58
 38  \w     29.00  70.00   0.50    0.10    --   63.87 -95.00 120.00   82
 39  \w     32.00  69.00   0.50    0.10    --   63.87 -95.00-180.00   74
 40  \w     62.00  87.00   0.50    0.10    --   75.73 153.00-165.00   50
 41  \w     63.00  88.00   0.50    0.10    --   76.61 153.00-165.00   50
 42  \w     47.00 115.00   0.50    0.10    --   79.75   6.00 -59.88  136
 43  \w     66.00  92.00   0.50    0.10    --   79.75  21.00-124.81   52
 44  \w     69.00 123.00   0.50    0.10    --   79.75  22.00  76.81  108
 45  \w     91.00 116.00   0.50    0.10    --   79.75  22.00 134.41   50
 46  \w     64.00 127.00   0.50    0.10    --   79.75  22.00 107.38  126
 47  \w     58.00  83.00   0.50    0.10    --   79.75  19.00  65.75   50
 48  \w     94.00 120.00   0.50    0.10    --   79.75  19.00  65.75   52
 49  \w     61.00 123.00   0.50    0.10    --   79.75  10.00  17.73  124
;
_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      -0.0008735000
_diffrn_orient_matrix_UB_12      -0.0830979000
_diffrn_orient_matrix_UB_13      -0.0138092000
_diffrn_orient_matrix_UB_21      -0.1085796000
_diffrn_orient_matrix_UB_22      0.0090391000
_diffrn_orient_matrix_UB_23      -0.0713156000
_diffrn_orient_matrix_UB_31      0.1008881000
_diffrn_orient_matrix_UB_32      0.0089743000
_diffrn_orient_matrix_UB_33      -0.0556646000
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.625
_diffrn_reflns_theta_min         3.565
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.118
_exptl_absorpt_correction_T_max  0.759
_exptl_absorpt_correction_T_min  0.473
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.130a (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            'clear intense orange'
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       prism
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.448
_refine_diff_density_min         -1.008
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         6598
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0423P)^2^+6.8536P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6040
_reflns_number_total             6598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc04154f2.cif
_cod_data_source_block           ga-189-ir-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_database_code               7134977
_shelx_shelxl_version_number     2019/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C64 H98 Cl4 Ir2 Li2 O3 P2'
_shelx_estimated_absorpt_t_max   0.688
_shelx_estimated_absorpt_t_min   0.463
_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. Restrained distances
 O2-C31 = O2-C34
 1.44 with sigma of 0.01
 C31-C32 = C33-C34
 1.53 with sigma of 0.01
 C32-C33
 1.54 with sigma of 0.01
 O2-C32 = O2-C33 = C31-C33 = C32-C34
 2.38 with sigma of 0.01
 C22A-C21 \\sim C22B-C21 \\sim C30A-C21 \\sim C29B-C21 \\sim C29A-C21 \\sim
C30B-C21
 with sigma of 0.02
 C23A-C22A \\sim C23B-C22B \\sim C30A-C25A \\sim C25B-C29B \\sim C29A-C27A
\\sim C27B-C30B
 with sigma of 0.02
 C28A-C27A \\sim C26A-C27A \\sim C28B-C23B \\sim C23B-C24B \\sim C25A-C24A
\\sim C24A-C23A \\sim C27B-
 C26B \\sim C25B-C26B \\sim C25A-C26A \\sim C27B-C28B \\sim C24B-C25B \\sim
C28A-C23A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C22A \\sim C22B \\sim C23A \\sim C23B \\sim C24A \\sim C24B \\sim C25A \\sim
C25B \\sim C26A \\sim C26B \\sim C27A \\sim C27B \\sim C28A \\sim C28B \\sim
C29A \\sim C29B \\sim C30A \\sim C30B: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2A
O2 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
4. Others
 Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24C)=
 Sof(H24D)=Sof(C25B)=Sof(H25B)=Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=
 Sof(H27B)=Sof(C28B)=Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=Sof(H29D)=
 Sof(C30B)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(C30A)=Sof(H30A)=Sof(H30B)=FVAR(1)
 Fixed Sof: O2(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5) H34B(0.5)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C15(H15), C18(H18), C23A(H23A), C23B(H23B), C25A(H25A), C25B(H25B),
 C27A(H27A), C27B(H27B)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A,
 H19B), C20(H20A,H20B), C22A(H22A,H22B), C22B(H22C,H22D), C24A(H24A,H24B),
 C24B(H24C,H24D), C26A(H26A,H26B), C26B(H26C,H26D), C28A(H28A,H28B), C28B(H28C,
 H28D), C29A(H29A,H29B), C29B(H29C,H29D), C30A(H30A,H30B), C30B(H30C,H30D),
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C)
;
_shelx_res_checksum              78698
_shelx_hkl_checksum              25789
_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 1.402
_oxdiff_exptl_absorpt_empirical_full_min 0.905