Diphosphaenones: beyond the phosphorus analogue of enones.
Lin, Jieli; Liu, Shihua; Zheng, Shunlin; Grützmacher, Hansjörg; Su, Cheng-Yong; Li, Zhongshu; Chemical science 15 (2024) 20030–20038; doi:10.1039/d4sc06462c

data_1573089
_publ_section_title
;
 Diphosphaenones: beyond the phosphorus analogue of enones.
;
_journal_issue                   47
_journal_name_full               'Chemical science'
_journal_page_first              20030
_journal_page_last               20038
_journal_paper_doi               10.1039/d4sc06462c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C63 H96 K N5 O P2 Si2, C6 H4 F'
_chemical_formula_sum            'C69 H100 F K N5 O P2 Si2'
_chemical_formula_weight         1191.75
_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             2024-02-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-27 deposited with the CCDC.	2024-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                98.712(2)
_cell_angle_beta                 103.862(2)
_cell_angle_gamma                98.212(2)
_cell_formula_units_Z            2
_cell_length_a                   12.0896(6)
_cell_length_b                   16.0159(8)
_cell_length_c                   21.5597(11)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      59.228
_cell_measurement_theta_min      2.797
_cell_volume                     3935.8(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74751
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         59.441
_diffrn_reflns_theta_min         1.871
_diffrn_source_current           3.57
_diffrn_source_power             0.24947159999999996
_diffrn_source_voltage           69.88
_exptl_absorpt_coefficient_mu    1.038
_exptl_absorpt_correction_T_max  0.2081
_exptl_absorpt_correction_T_min  0.1096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1621 before and 0.0666 after correction.
The Ratio of minimum to maximum transmission is 0.5267.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_description       block
_exptl_crystal_F_000             1286
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         17203
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.5728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13072
_reflns_number_total             17203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06462c2.cif
_cod_data_source_block           10a
_cod_depositor_comments
'Adding full bibliography for 1573084--1573090.cif.'
_cod_database_code               1573089
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.860
_olex2_refinement_description
;
1. Rigid bond restraints
 Si2, C6, C7, C8
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
2. Uiso/Uaniso restraints and constraints
Si2 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.005 within 2A
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H64(0.2) H69(0.4) H68(0.4) F1(0.4) F2(0.2) F3(0.4)
4.a Ternary CH refined with riding coordinates:
 C23(H23), C62(H62), C35(H35), C26(H26), C59(H59), C38(H38), C47(H47), C50(H50)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C12(H12A,H12B), C15(H15A,H15B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C2(H2), C32(H32), C55(H55), C30(H30), C54(H54), C31(H31), C56(H56),
 C20(H20), C19(H19), C18(H18), C44(H44), C65(H65), C42(H42), C43(H43), C64(H64),
  C66(H66), C69(H69), C67(H67), C68(H68)
4.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C10(H10A,H10B,
 H10C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C60(H60A,H60B,
 H60C), C34(H34A,H34B,H34C), C61(H61A,H61B,H61C), C36(H36A,H36B,H36C), C58(H58A,
 H58B,H58C), C48(H48A,H48B,H48C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C),
 C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C51(H51A,H51B,H51C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'