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_7034194
_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         'C33 H46 N2 O P2'
_chemical_formula_sum            'C33 H46 N2 O P2'
_chemical_formula_weight         548.66
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-29
_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                90
_cell_angle_beta                 93.823(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3904(5)
_cell_length_b                   20.3999(9)
_cell_length_c                   13.5469(6)
_cell_measurement_reflns_used    8864
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      43.007
_cell_measurement_theta_min      3.923
_cell_volume                     3140.8(2)
_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      100.8
_diffrn_measured_fraction_theta_full 0.873
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1555
_diffrn_reflns_av_unetI/netI     0.0835
_diffrn_reflns_Laue_measured_fraction_full 0.873
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18429
_diffrn_reflns_point_group_measured_fraction_full 0.873
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.937
_diffrn_reflns_theta_min         3.923
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.453
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         4958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0774
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+7.8983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.1971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3984
_reflns_number_total             4958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt04012k2.cif
_cod_data_source_block           cu_ppco_ene1_0m
_cod_depositor_comments
'Adding full bibliography for 7034191--7034195.cif.'
_cod_database_code               7034194
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O1A)=1-FVAR(1)
 Sof(O1)=FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(N2A)=Sof(H2A)=1-FVAR(2)
 Sof(N2)=Sof(H2)=Sof(C1)=Sof(H1)=FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=
 Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(3)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C31)=Sof(H31)=Sof(C33)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=FVAR(3)
 Sof(C28A)=Sof(H28A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C29A)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(4)
 Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=FVAR(4)
3.a Ternary CH refined with riding coordinates:
 C19(H19), C16(H16), C28(H28), C31(H31), C31A(H31A), C28A(H28A)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C13(H13), C12(H12), C26(H26), C24(H24), C25(H25), N2(H2), C1(H1),
 C1A(H1A), N2A(H2A)
3.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C21(H21A,H21B,H21C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C32A(H32D,H32E,H32F),
 C33A(H33D,H33E,H33F), C30A(H30D,H30E,H30F), C29A(H29D,H29E,H29F)
;
_olex2_submission_special_instructions 'No special instructions were received'