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_1573088
_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         'C64 H96 N4 O2 P2 Si, C2 H3 N'
_chemical_formula_sum            'C66 H99 N5 O2 P2 Si'
_chemical_formula_weight         1084.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-09-22 deposited with the CCDC.	2024-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.6100(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5772(2)
_cell_length_b                   16.1173(2)
_cell_length_c                   21.8954(2)
_cell_measurement_reflns_used    45651
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      51.7120
_cell_measurement_theta_min      2.0680
_cell_volume                     6463.80(12)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -19.00  73.00   0.50    6.00    --   -0.70  58.00  73.00  184
  2  \w    -15.00  69.00   0.50   10.00    --   57.04 -58.00 -67.00  168
  3  \w     38.00 131.00   0.50   10.00    --   57.04  58.00  73.00  186
  4  \w   -131.00 -40.00   0.50   10.00    --  -58.45 -58.00 -67.00  182
  5  \w    -65.00  15.00   0.50   10.00    --  -58.45  58.00  73.00  160
  6  \w    -74.00  18.00   0.50    6.00    --   -0.70 -57.00 150.00  184
  7  \w    -76.00  18.00   0.50    6.00    --   -0.70 -38.00 -60.00  188
  8  \w    -74.00  18.00   0.50    6.00    --   -0.70 -58.00 -67.00  184
  9  \w    -17.00  35.00   0.50    6.00    --   -0.70 -99.00-150.00  104
 10  \w    -20.00  28.00   0.50   10.00    --   57.04 -19.00 -60.00   96
 11  \w    -18.00  45.00   0.50   10.00    --   57.04 -38.00 -60.00  126
 12  \w     80.00 128.00   0.50   10.00    --   57.04 125.00   0.00   96
 13  \w    -18.00  45.00   0.50   10.00    --   57.04 -38.00 120.00  126
 14  \w     39.00 132.00   0.50   10.00    --   57.04  38.00  60.00  186
 15  \w    -15.00  68.00   0.50   10.00    --   57.04 -57.00 -30.00  166
 16  \w    -18.00  45.00   0.50   10.00    --   57.04 -38.00 150.00  126
 17  \w     39.00 127.00   0.50   10.00    --   57.04  38.00-180.00  176
 18  \w     81.00 127.00   0.50   10.00    --   57.04 125.00-120.00   92
 19  \w     81.00 107.00   0.50   10.00    --   57.04 125.00 150.00   52
 20  \w     39.00  95.00   0.50   10.00    --   57.04  38.00-120.00  112
 21  \w    103.00 132.00   0.50   10.00    --   57.04  38.00-120.00   58
 22  \w    -20.00  28.00   0.50   10.00    --   57.04 -19.00   0.00   96
 23  \w   -136.00 -37.00   0.50   10.00    --  -58.45 -19.00 120.00  198
 24  \w    -24.00  20.00   0.50   10.00    --  -58.45  19.00 150.00   88
 25  \w    -44.00   6.00   0.50   10.00    --  -58.45  57.00-150.00  100
 26  \w    -16.00  17.00   0.50   10.00    --  -58.45  19.00-150.00   66
 27  \w   -131.00 -43.00   0.50   10.00    --  -58.45 -57.00-120.00  176
 28  \w    -16.00  19.00   0.50   10.00    --  -58.45  19.00-180.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0362330000
_diffrn_orient_matrix_UB_12      -0.0654595000
_diffrn_orient_matrix_UB_13      -0.0464957000
_diffrn_orient_matrix_UB_21      -0.0658485000
_diffrn_orient_matrix_UB_22      -0.0038589000
_diffrn_orient_matrix_UB_23      0.0343722000
_diffrn_orient_matrix_UB_31      -0.0377759000
_diffrn_orient_matrix_UB_32      0.0695174000
_diffrn_orient_matrix_UB_33      -0.0418321000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            67186
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        51.823
_diffrn_reflns_theta_max         51.823
_diffrn_reflns_theta_min         2.892
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       plate
_exptl_crystal_F_000             2360
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         7107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0370P)^2^+4.5268P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6582
_reflns_number_total             7107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06462c2.cif
_cod_data_source_block           7b
_cod_depositor_comments
'Adding full bibliography for 1573084--1573090.cif.'
_cod_database_code               1573088
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     CHON
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.935
_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.a Ternary CH refined with riding coordinates:
 C25(H25), C22(H22), C63(H63), C51(H51), C34(H34), C37(H37), C60(H60), C48(H48)
2.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C40(H40A,H40B), C14(H14A,H14B), C39(H39A,H39B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C17(H17), C29(H29), C4(H4), C31(H31), C18(H18), C30(H30), C58(H58),
 C19(H19), C43(H43), C55(H55), C45(H45), C56(H56), C44(H44)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C), C52(H52A,H52B,
 H52C), C50(H50A,H50B,H50C), C12(H12A,H12B,H12C), C33(H33A,H33B,H33C), C38(H38A,
 H38B,H38C), C9(H9A,H9B,H9C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C),
 C61(H61A,H61B,H61C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C), C59(H59A,H59B,
 H59C), C49(H49A,H49B,H49C), C10(H10A,H10B,H10C), C35(H35A,H35B,H35C), C23(H23A,
 H23B,H23C), C8(H8A,H8B,H8C), C47(H47A,H47B,H47C), C7(H7A,H7B,H7C), C66(H66A,
 H66B,H66C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.543
_oxdiff_exptl_absorpt_empirical_full_min 0.475