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_7034191
_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         'C53 H72 N4 O P4'
_chemical_formula_sum            'C53 H72 N4 O P4'
_chemical_formula_weight         905.02
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-29
_audit_creation_method
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Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
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_audit_update_record
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2015-02-07 deposited with the CCDC.
2015-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                68.043(2)
_cell_angle_beta                 77.0428(17)
_cell_angle_gamma                73.5767(17)
_cell_formula_units_Z            2
_cell_length_a                   9.86749(18)
_cell_length_b                   15.8674(3)
_cell_length_c                   18.6581(4)
_cell_measurement_reflns_used    27582
_cell_measurement_temperature    105(1)
_cell_measurement_theta_max      32.4140
_cell_measurement_theta_min      3.1650
_cell_volume                     2575.72(10)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      105(1)
_diffrn_detector_area_resol_mean 16.0839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details
;
  1 omega  -78.00  -38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  125.0000 -155.0000 40

  2 omega  -74.00  -46.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  179.0000  -60.0000 28

  3 omega  -95.00  -39.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865  -57.0000   90.0000 56

  4 omega   17.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000   30.0000 51

  5 omega  -16.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -99.0000  150.0000 84

  6 omega  -43.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -19.0000  150.0000 114

  7 omega    9.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   57.0000  -30.0000 87

  8 omega -103.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865 -179.0000 -150.0000 69

  9 omega    6.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   57.0000 -180.0000 90

 10 omega  -42.00   48.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -57.0000   60.0000 90

 11 omega   -3.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   77.0000  -60.0000 100

 12 omega   -3.00   97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   77.0000   60.0000 100

 13 omega    6.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   57.0000 -150.0000 90

 14 omega -103.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865 -179.0000   90.0000 69

 15 omega -103.00  -34.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.3865 -179.0000  -90.0000 69

 16 omega  -46.00   52.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553  -38.0000 -180.0000 98

 17 omega   -3.00   22.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8553   77.0000  -90.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0058878000
_diffrn_orient_matrix_UB_12      -0.0050683000
_diffrn_orient_matrix_UB_13      0.0399218000
_diffrn_orient_matrix_UB_21      -0.0049990000
_diffrn_orient_matrix_UB_22      0.0484756000
_diffrn_orient_matrix_UB_23      -0.0103474000
_diffrn_orient_matrix_UB_31      -0.0752185000
_diffrn_orient_matrix_UB_32      0.0081047000
_diffrn_orient_matrix_UB_33      0.0031009000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82945
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.569
_diffrn_reflns_theta_min         2.843
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.167
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         17517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0623P)^2^+1.1412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1274
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15657
_reflns_number_total             17517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt04012k2.cif
_cod_data_source_block           exp_2571
_cod_depositor_comments
'Adding full bibliography for 7034191--7034195.cif.'
_cod_original_cell_volume        2575.71(10)
_cod_database_code               7034191
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         C10H10N2P2O2
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C38(H38A,H38B,H38C), C7(H7A,H7B,H7C),
 C12(H12A,H12B,H12C), C26(H26A,H26B,H26C), C51(H51A,H51B,H51C), C21(H21A,H21B,
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 H36B,H36C), C23(H23A,H23B,H23C), C41(H41A,H41B,H41C), C50(H50A,H50B,H50C)
;
_olex2_submission_special_instructions 'No special instructions were received'