The case of a μ<sub>2</sub>-P aromatic phosphinine as a 4-electron donor forming σ- and π-three-center-two-electron bonds.
Zhang, Jie; Hou, Yuanfeng; Liu, Shihua; Lin, Jieli; Li, Zhongshu; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5608–5615; doi:10.1039/d4dt00228h

data_7715205
_publ_section_title
;
 The case of a &#x3bc;<sub>2</sub>-P aromatic phosphinine as a 4-electron
 donor forming &#x3c3;- and &#x3c0;-three-center-two-electron bonds.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5608
_journal_page_last               5615
_journal_paper_doi               10.1039/d4dt00228h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C102 H72 O6 P8 Rh2, 6(C4 H8 O)'
_chemical_formula_sum            'C126 H120 O12 P8 Rh2'
_chemical_formula_weight         2279.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-09-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-10-20 deposited with the CCDC.	2024-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.9920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.87110(10)
_cell_length_b                   33.0914(3)
_cell_length_c                   21.7367(2)
_cell_measurement_reflns_used    25199
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      73.8630
_cell_measurement_theta_min      2.9760
_cell_volume                     10728.12(17)
_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 0.999
_diffrn_measured_fraction_theta_max 0.971
_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    -86.00 -35.00   0.50    3.05    --    0.00 -77.00 -90.00  102
  2  \w    -18.00  53.00   0.50    3.05    --    0.00  57.00 120.00  142
  3  \w      7.00  84.00   0.50    3.05    --    0.00  38.00 -60.00  154
  4  \w     80.00 109.00   0.50   12.21    --   95.20 -45.00 -30.00   58
  5  \w      7.00  74.00   0.50   12.21    --   95.20 -77.00  60.00  134
  6  \w     80.00 107.00   0.50   12.21    --   95.20 -77.00  60.00   54
  7  \w      6.00 103.00   0.50   12.21    --   95.20 -61.00  90.00  194
  8  \w     65.00 107.00   0.50   12.21    --   95.20 -77.00 -90.00   84
  9  \w      6.00  55.00   0.50   12.21    --   95.20 -77.00 -90.00   98
 10  \w      6.00 109.00   0.50   12.21    --   95.20 -30.00 120.00  206
 11  \w     17.00 108.00   0.50   12.21    --   95.20 -30.00 -90.00  182
 12  \w      6.00  36.00   0.50   12.21    --   95.20 -45.00 -30.00   60
 13  \w     83.00 109.00   0.50   12.21    --   95.20  45.00-150.00   52
 14  \w     97.00 185.00   0.50   12.21    --   95.20  30.00-150.00  176
;
_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      0.0410263000
_diffrn_orient_matrix_UB_12      0.0307042000
_diffrn_orient_matrix_UB_13      0.0554577000
_diffrn_orient_matrix_UB_21      0.0918321000
_diffrn_orient_matrix_UB_22      -0.0048776000
_diffrn_orient_matrix_UB_23      -0.0086374000
_diffrn_orient_matrix_UB_31      -0.0233769000
_diffrn_orient_matrix_UB_32      0.0346786000
_diffrn_orient_matrix_UB_33      -0.0503470000
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            66736
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.148
_diffrn_reflns_theta_min         2.542
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80890
_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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.246
_refine_diff_density_min         -1.616
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1360
_refine_ls_number_reflns         21196
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+52.4713P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17428
_reflns_number_total             21196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00228h2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7715202--7715205.cif.'
_cod_database_code               7715205
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.637
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C115-C116
 1.45 with sigma of 0.02
 C112-C111
 1.6 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C130) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C126) \\sim Ueq,
Uanis(C129) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(O12)
\\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(C123) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C115) \\sim Ueq, Uanis(C116) \\sim Ueq, Uanis(C117) \\sim Ueq,
Uanis(C118) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(C114)
\\sim Ueq, Uanis(C113) \\sim Ueq, Uanis(C111) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C125(0.5) H12G(0.5) H12H(0.5) C124(0.5) H12J(0.5) H12I(0.5)
 C130(0.5) H13A(0.5) H13B(0.5) O12(0.5) C127(0.5) H12K(0.5) H12L(0.5) C128(0.5)
 H12M(0.5) H12N(0.5) C126(0.5) H12O(0.5) H12P(0.5) O13(0.5) C123(0.5) H12Q(0.5)
 H12R(0.5) C129(0.5) H12T(0.5) H12S(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C103(H10K,H10L), C104(H10J,H10I), C105(H10M,H10N), C106(H10G,H10H), C107(H10A,
 H10B), C108(H10C,H10D), C109(H10E,H10F), C110(H11A,H11B), C111(H11C,H11D),
 C112(H11E,H11F), C113(H11I,H11J), C114(H11G,H11H), C115(H11S,H11T), C116(H11M,
 H11N), C117(H11O,H11P), C118(H11Q,H11R), C119(H11K,H11L), C120(H12E,H12F),
 C121(H12A,H12B), C122(H12C,H12D), C125(H12G,H12H), C124(H12J,H12I), C130(H13A,
 H13B), C127(H12K,H12L), C128(H12M,H12N), C126(H12O,H12P), C123(H12Q,H12R),
 C129(H12T,H12S)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C9(H9), C12(H12), C14(H14), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C37(H37),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
 C58(H58), C60(H60), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C69(H69),
  C70(H70), C71(H71), C72(H72), C73(H73), C75(H75), C76(H76), C77(H77),
 C78(H78), C79(H79), C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C87(H87),
  C89(H89), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C98(H98),
 C99(H99), C100(H100), C101(H101), C102(H102)
5.c Fitted pentagon refined as free rotating group:
 C125(C124,C130,O12,C127), C128(C126,O13,C123,C129)
;
_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 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.787