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_1573084
_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         'C57 H78 N4 O P2'
_chemical_formula_sum            'C57 H78 N4 O P2'
_chemical_formula_weight         897.17
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-20
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.95760(10)
_cell_length_b                   27.95760(10)
_cell_length_c                   15.51230(10)
_cell_measurement_reflns_used    37769
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.9300
_cell_measurement_theta_min      3.1650
_cell_volume                     12124.84(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_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    -48.00 -22.00   0.50    0.50    --    0.00   0.00 150.00   52
  2  \w      4.00  88.00   0.50    0.50    --    0.00   0.00 150.00  168
  3  \w     15.00  88.00   0.50    0.50    --    0.00  38.00-150.00  146
  4  \w    -37.00   2.00   0.50    0.50    --    0.00 -57.00   0.00   78
  5  \w     58.00 115.00   0.50    1.92    --   95.20 -45.00 -30.00  114
  6  \w      9.00  81.00   0.50    1.92    --   95.20 -77.00-120.00  144
  7  \w     79.00 140.00   0.50    1.92    --   95.20  45.00  90.00  122
  8  \w     11.00  71.00   0.50    1.92    --   95.20 -77.00 -60.00  120
  9  \w      8.00  37.00   0.50    1.92    --   95.20 -45.00 -30.00   58
 10  \w     87.00 124.00   0.50    1.92    --   95.20 -77.00 -60.00   74
 11  \w     86.00 163.00   0.50    1.92    --   95.20  30.00-180.00  154
 12  \w     76.00 102.00   0.50    1.92    --   95.20  15.00 120.00   52
 13  \w    129.00 177.00   0.50    1.92    --   95.20  15.00 120.00   96
 14  \w     84.00 125.00   0.50    1.92    --   95.20 -77.00-120.00   82
 15  \w     87.00 178.00   0.50    1.92    --   95.20  30.00 150.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0390085000
_diffrn_orient_matrix_UB_12      -0.0386095000
_diffrn_orient_matrix_UB_13      0.0088292000
_diffrn_orient_matrix_UB_21      -0.0259545000
_diffrn_orient_matrix_UB_22      -0.0206253000
_diffrn_orient_matrix_UB_23      0.0792980000
_diffrn_orient_matrix_UB_31      -0.0290372000
_diffrn_orient_matrix_UB_32      -0.0334194000
_diffrn_orient_matrix_UB_33      -0.0591719000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            73809
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.329
_diffrn_reflns_theta_min         3.161
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.983
_exptl_crystal_description       block
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details
;
 Flack x determined using 5105 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         12206
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0330
_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^)+(0.0495P)^2^+1.1830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0904
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                11725
_reflns_number_total             12206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc06462c2.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 1573084--1573090.cif.'
_cod_original_cell_volume        12124.84(12)
_cod_database_code               1573084
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.852
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C27(H27), C30(H30), C41(H41), C44(H44), C53(H53), C56(H56)
1.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C32(H32A,H32B), C33(H33A,H33B)
1.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C10(H10), C11(H11), C12(H12), C22(H22), C23(H23), C24(H24),
 C36(H36), C37(H37), C38(H38), C48(H48), C49(H49), C50(H50)
1.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,
 H31B,H31C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C),
 C45(H45A,H45B,H45C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C57(H57A,H57B,H57C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.254
_oxdiff_exptl_absorpt_empirical_full_min 0.401