Arbuzov meets 1,2-oxaphosphetanes: transient 1,2-oxaphosphetan-2-iums as an entry point to beta-halo phosphane oxides and P-containing oligomers.
Gleim, Florian; Schnakenburg, Gregor; Ferao, Arturo Espinosa; Streubel, Rainer; Chemical communications (Cambridge, England) 60 (2024) 2625–2628; doi:10.1039/d4cc00254g

data_7132685
_publ_section_title
;
 Arbuzov meets 1,2-oxaphosphetanes: transient 1,2-oxaphosphetan-2-iums as
 an entry point to beta-halo phosphane oxides and P-containing oligomers.
;
_journal_issue                   19
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2625
_journal_page_last               2628
_journal_paper_doi               10.1039/d4cc00254g
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C28 H23 Mo O6 P'
_chemical_formula_sum            'C28 H23 Mo O6 P'
_chemical_formula_weight         582.37
_chemical_name_systematic        FLG-308
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-08-22 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                99.296(2)
_cell_angle_beta                 92.701(2)
_cell_angle_gamma                95.011(2)
_cell_formula_units_Z            6
_cell_length_a                   9.4957(6)
_cell_length_b                   18.3164(14)
_cell_length_c                   22.5419(16)
_cell_measurement_reflns_used    7002
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      2.30
_cell_volume                     3846.9(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      100.0
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.929
_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  0.0630
_diffrn_reflns_av_unetI/netI     0.1744
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_number            17274
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.834
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.745985
_exptl_absorpt_correction_T_min  0.599645
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 102432 reflections, Rint = 0.1156
 (23683 with I > 3sig(I), Rint = 0.0630)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.232
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         17274
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0785P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9763
_reflns_number_total             17274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00254g2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7132681--7132686.cif.'
_cod_database_code               7132685
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.709
_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
Uanis(C28) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C28A)
\\sim Ueq, Uanis(C26A) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2'(H2'A,H2'B), C2A(H2AA,H2AB)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C7'(H7'),
  C8'(H8'), C9'(H9'), C10'(H10'), C11'(H11'), C13'(H13'), C14'(H14'),
 C15'(H15'), C16'(H16'), C17'(H17'), C19'(H19'), C20'(H20'), C21'(H21'),
 C22'(H22'), C23'(H23'), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A),
 C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C19A(H19A),
 C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C3'(H3'A,H3'B,H3'C), C4'(H4'A,H4'B,H4'C),
 C3A(H3AA,H3AB,H3AC), C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              56838
_shelx_hkl_checksum              54225
_olex2_submission_special_instructions 'No special instructions were received'