Oxaphosphiranes: isolable phosphorus-containing epoxide rings.
Volk, Niklas; García Alcaraz, Antonio; Balasubramaniam, Selvakumar; Heumann, Jannik; Schnakenburg, Gregor; Espinosa Ferao, Arturo; Streubel, Rainer; Dalton transactions (Cambridge, England : 2003) 53 (2024) 19351–19359; doi:10.1039/d4dt02915a

data_7717329
_publ_section_title
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 Oxaphosphiranes: isolable phosphorus-containing epoxide rings.
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_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19351
_journal_page_last               19359
_journal_paper_doi               10.1039/d4dt02915a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C31 H28 N2 O5 P W'
_chemical_formula_sum            'C31 H28 N2 O5 P W'
_chemical_formula_weight         723.37
_chemical_name_systematic        SB-66
_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   mixed
_audit_creation_date             2024-09-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
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2024-09-05 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.581(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3149(3)
_cell_length_b                   22.2032(9)
_cell_length_c                   13.9550(6)
_cell_measurement_reflns_used    9668
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.517
_cell_measurement_theta_min      2.353
_cell_volume                     2860.95(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            59659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.389
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    4.136
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1165 before and 0.0500 after correction. The Ratio of minimum to maximum transmission is 0.7518. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       plank
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0157
_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^)+(0.0138P)^2^+2.6429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0382
_refine_ls_wR_factor_ref         0.0387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6605
_reflns_number_total             6918
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02915a2.cif
_cod_data_source_block           19
_cod_depositor_comments
'Adding full bibliography for 7717326--7717330.cif.'
_cod_database_code               7717329
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.852
_shelx_estimated_absorpt_t_min   0.437
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, H of C31
 At 1.2 times of:
  H10 of C10, H25 of C25, H23 of C23, H13 of C13, H12 of C12, H14 of C14, H11
  of C11, H17 of C17, H18 of C18, H22 of C22, H24 of C24, H16 of C16, H20 of
  C20, H26 of C26, H19 of C19
2.a Me refined with riding coordinates:
 C7(H7A,H7B,H7C)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              20059
_shelx_hkl_checksum              66724
_olex2_submission_special_instructions 'No special instructions were received'