[2 + 2] Cycloaddition of phosphaalkenes as a key step for the reductive coupling of diaryl ketones to tetraaryl olefins
Arkhypchuk, Anna I.; D'Imperio, Nicolas; Wells, Jordann A. L.; Ott, Sascha; Chemical Science 13 (2022) 12239–12244; doi:10.1039/D2SC03073J

data_1567698
_publ_section_title
;
 [2 + 2] Cycloaddition of phosphaalkenes as a key step for the reductive
 coupling of diaryl ketones to tetraaryl olefins
;
_journal_issue                   41
_journal_name_full               'Chemical Science'
_journal_page_first              12239
_journal_page_last               12244
_journal_paper_doi               10.1039/D2SC03073J
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C H Cl3, C32 H28 F2 O2'
_chemical_formula_sum            'C33 H29 Cl3 F2 O2'
_chemical_formula_weight         601.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-25 deposited with the CCDC.	2022-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_measurement_theta_max      21.58
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_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1726 before and 0.0415 after correction. The Ratio of minimum to maximum transmission is 0.9353. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
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_refine_ls_extinction_method     none
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.1472P)^2^+3.6384P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2567
_refine_ls_wR_factor_ref         0.2958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4042
_reflns_number_total             6053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc03073j2.cif
_cod_data_source_block           so2009
_cod_depositor_comments
'Adding full bibliography for 1567695--1567699.cif.'
_cod_original_cell_volume        3074.1(13)
_cod_database_code               1567698
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.884
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1S(H)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C9(H9A,H9B), C11(H11A,H11B), C14(H14A,H14B), C13(H13A,H13B),
 C10(H10A,H10B)
2.c Aromatic/amide H refined with riding coordinates:
 C32(H32), C7(H7), C17(H17), C5(H5), C8(H8), C20(H20), C4(H4), C19(H19),
 C16(H16), C28(H28), C31(H31), C22(H22), C26(H26), C29(H29), C25(H25), C23(H23)
;
_shelx_res_checksum              44641
_shelx_hkl_checksum              90913
_olex2_submission_special_instructions 'No special instructions were received'