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_7132686
_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         'C29 H26 Br O2 P'
_chemical_formula_sum            'C29 H26 Br O2 P'
_chemical_formula_weight         517.38
_chemical_name_systematic        FLG-350
_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
_audit_creation_date             2022-04-22
_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                69.469(6)
_cell_angle_beta                 84.259(7)
_cell_angle_gamma                72.909(7)
_cell_formula_units_Z            2
_cell_length_a                   8.9276(15)
_cell_length_b                   10.5777(17)
_cell_length_c                   14.307(2)
_cell_measurement_reflns_used    6318
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      3.02
_cell_volume                     1209.4(3)
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_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  0.1078
_diffrn_reflns_av_unetI/netI     0.1317
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4735
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.140
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  0.746069
_exptl_absorpt_correction_T_min  0.487803
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 38358 reflections, Rint = 0.2247
 (11914 with I > 3sig(I), Rint = 0.1078)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_description       needle
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.482
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4735
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1510
_refine_ls_R_factor_gt           0.0874
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0751P)^2^+16.3100P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2096
_refine_ls_wR_factor_ref         0.2394
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3735
_reflns_number_total             4735
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc00254g2.cif
_cod_data_source_block           10b
_cod_depositor_comments
'Adding full bibliography for 7132681--7132686.cif.'
_cod_database_code               7132686
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.634
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.733(3)
 0.267(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C9(H9A,H9B), C10(H10A,H10B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
  C26(H26), C27(H27), C28(H28), C29(H29)
;
_shelx_res_checksum              91329
_shelx_hkl_checksum              38523
_olex2_submission_special_instructions 'No special instructions were received'