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_7717327
_publ_section_title
;
 Oxaphosphiranes: isolable phosphorus-containing epoxide rings.
;
_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 H19 F2 O6 P W'
_chemical_formula_sum            'C31 H19 F2 O6 P W'
_chemical_formula_weight         740.28
_chemical_name_systematic        NV-445
_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
_audit_creation_date             2021-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-09-05 deposited with the CCDC.	2024-10-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.453(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0720(12)
_cell_length_b                   9.5515(4)
_cell_length_c                   16.6957(9)
_cell_measurement_reflns_used    5275
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.66
_cell_volume                     2790.1(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.1350
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14278
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.660
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    4.254
_exptl_absorpt_correction_T_max  0.8557
_exptl_absorpt_correction_T_min  0.3478
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       plate
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.977
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.756
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6616
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.757
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0145P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0600
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3935
_reflns_number_total             6616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02915a2.cif
_cod_data_source_block           3c
_cod_depositor_comments
'Adding full bibliography for 7717326--7717330.cif.'
_cod_database_code               7717327
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.404
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C6) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C24)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), 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)
;
_shelx_res_checksum              69232
_shelx_hkl_checksum              72700
_olex2_submission_special_instructions 'No special instructions were received'