A stable phosphanyl phosphaketene and its reactivity.
Li, Zhongshu; Chen, Xiaodan; Bergeler, Maike; Reiher, Markus; Su, Cheng-Yong; Grützmacher, Hansjörg; Dalton transactions (Cambridge, England : 2003) 44 (2015) 6431–6438; doi:10.1039/c4dt04012k

data_7034195
_publ_section_title
;
 A stable phosphanyl phosphaketene and its reactivity.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6431
_journal_page_last               6438
_journal_paper_doi               10.1039/c4dt04012k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C57 H56 O P2, 3(C2 H3 N)'
_chemical_formula_sum            'C63 H65 N3 O P2'
_chemical_formula_weight         942.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-07 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                73.099(3)
_cell_angle_beta                 63.618(3)
_cell_angle_gamma                71.027(3)
_cell_formula_units_Z            4
_cell_length_a                   17.7901(14)
_cell_length_b                   18.7231(16)
_cell_length_c                   19.1169(16)
_cell_measurement_reflns_used    9744
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.311
_cell_measurement_theta_min      2.336
_cell_volume                     5313.5(8)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.7
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            243043
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.355
_diffrn_reflns_theta_min         2.123
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_type   none
_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    1.178
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1239
_refine_ls_number_reflns         26447
_refine_ls_number_restraints     3205
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0844P)^2^+7.7838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20775
_reflns_number_total             26447
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt04012k2.cif
_cod_data_source_block           mo_ppco_diene_0m
_cod_depositor_comments
'Adding full bibliography for 7034191--7034195.cif.'
_cod_database_code               7034195
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 P1, C0AA
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P1, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, C4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P2, C8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C0AA \\sim C3 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim
C20 \\sim C23 \\sim C24 \\sim C25 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim
C32 \\sim C33 \\sim C35 \\sim C36 \\sim C38 \\sim C39 \\sim C43 \\sim C44 \\sim
C47 \\sim C48 \\sim C52 \\sim C57 \\sim C59 \\sim C60 \\sim C61 \\sim C63 \\sim
C65 \\sim C67 \\sim C68 \\sim C71 \\sim C72 \\sim C74 \\sim C75 \\sim C78 \\sim
C79 \\sim C80 \\sim C85 \\sim C91 \\sim C92 \\sim C94 \\sim C96 \\sim C97 \\sim
C98 \\sim C99 \\sim C101 \\sim C102 \\sim C107 \\sim C109 \\sim C110 \\sim C113
\\sim C121 \\sim C4 \\sim C5 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11
\\sim C12 \\sim C13 \\sim C21 \\sim C22 \\sim C26 \\sim C27 \\sim C34 \\sim C37
\\sim C40 \\sim C41 \\sim C42 \\sim C45 \\sim C46 \\sim C49 \\sim C50 \\sim C51
\\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C58 \\sim C62 \\sim C64 \\sim C66
\\sim C69 \\sim C70 \\sim C73 \\sim C76 \\sim C77 \\sim C81 \\sim C82 \\sim C83
\\sim C84 \\sim C86 \\sim C87 \\sim C88 \\sim C89 \\sim C90 \\sim C93 \\sim C95
\\sim C100 \\sim C103 \\sim C104 \\sim C105 \\sim C111 \\sim C112 \\sim C118
\\sim C119 \\sim C123 \\sim C125 \\sim C1 \\sim C2 \\sim C1B \\sim C6 \\sim C1C
\\sim C1A \\sim C1D \\sim C114 \\sim C117 \\sim C108 \\sim C115 \\sim C122
\\sim C127 \\sim C0AB \\sim C2A: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C119) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(N2A)=Sof(C0AB)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C2A)=1-FVAR(1)
 Sof(N2)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=FVAR(1)
 Sof(C1D)=1-FVAR(2)
 Sof(C1A)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C23(H23), C57(H57), C74(H74), C85(H85), C54(H54), C70(H70), C103(H103),
 C118(H118)
5.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C20(H20), C28(H28), C29(H29), C31(H31), C33(H33), C36(H36),
 C47(H47), C48(H48), C52(H52), C59(H59), C60(H60), C61(H61), C63(H63), C65(H65),
  C68(H68), C71(H71), C72(H72), C75(H75), C78(H78), C79(H79), C80(H80),
 C91(H91), C94(H94), C96(H96), C97(H97), C98(H98), C101(H101), C26(H26),
 C27(H27), C40(H40), C41(H41), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51),
  C55(H55), C56(H56), C58(H58), C62(H62), C64(H64), C66(H66), C69(H69),
 C73(H73), C76(H76), C77(H77), C82(H82), C83(H83), C84(H84), C87(H87), C89(H89),
  C93(H93), C95(H95), C104(H104), C112(H112)
5.c Idealised Me refined as rotating group:
 C92(H92A,H92B,H92C), C99(H99A,H99B,H99C), C102(H10A,H10B,H10C), C107(H10D,
 H10E,H10F), C109(H10G,H10H,H10I), C110(H11A,H11B,H11C), C113(H11D,H11E,H11F),
 C121(H12A,H12B,H12C), C81(H81A,H81B,H81C), C86(H86A,H86B,H86C), C100(H10J,H10K,
 H10L), C105(H10M,H10N,H10O), C111(H11G,H11H,H11I), C119(H11J,H11K,H11L),
 C123(H12D,H12E,H12F), C125(H12G,H12H,H12I), C1(H1A,H1B,H1C), C6(H6A,H6B,H6C),
 C1A(H1AA,H1AB,H1AC), C114(H11M,H11N,H11O), C108(H10P,H10Q,H10R), C127(H12J,
 H12K,H12L), C0AB(H0AA,H0AB,H0AC)
;
_olex2_submission_special_instructions 'No special instructions were received'