Generation and Trapping of a 1-Phosphafulvene: An Illustration of the P═C/C═C Analogy.
Hu, Zhengsong; Tian, Rongqiang; Zhao, Kang; Liu, Yanjie; Duan, Zheng; Mathey, François; Organic letters 19 (2017) 5004–5006; doi:10.1021/acs.orglett.7b02574

data_1547554
_publ_section_title
;
 Generation and Trapping of a 1-Phosphafulvene: An Illustration of the
 P&#x2550;C/C&#x2550;C Analogy.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              5004
_journal_page_last               5006
_journal_paper_doi               10.1021/acs.orglett.7b02574
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C26 H29 O P'
_chemical_formula_sum            'C26 H29 O P'
_chemical_formula_weight         388.46
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.050(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.3313(2)
_cell_length_b                   19.6104(5)
_cell_length_c                   15.1854(4)
_cell_measurement_reflns_used    5669
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.446
_cell_measurement_theta_min      3.695
_cell_volume                     2161.69(10)
_computing_cell_refinement
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb 1 2013,16:14:44)
;
_computing_data_collection
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb 1 2013,16:14:44)
;
_computing_data_reduction
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb 1 2013,16:14:44)
;
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.5281
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
 1 omega -116.00 -14.00 1.0000 1.0000
 omega____ theta____ kappa____ phi______ frames
 - -40.2335 -37.0000 120.0000 102
 2 omega 11.00 36.00 1.0000 1.0000
 omega____ theta____ kappa____ phi______ frames
 - -40.2335 37.0000 -90.0000 25
 3 omega -36.00 5.00 1.0000 1.0000
 omega____ theta____ kappa____ phi______ frames
 - -40.2335 37.0000 -90.0000 41
 4 omega -34.00 -4.00 1.0000 1.0000
 omega____ theta____ kappa____ phi______ frames
 - -40.2335 125.0000 -150.0000 30
 5 omega 27.00 54.00 1.0000 1.0000
 omega____ theta____ kappa____ phi______ frames
 - 40.2335 -125.0000 30.0000 27
 6 omega -35.00 11.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - -61.5000 45.0000 30.0000 46
 7 omega 136.00 173.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 111.0000 0.0000 37
 8 omega 147.00 176.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 15.0000 -90.0000 29
 9 omega 39.00 65.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -45.0000 90.0000 26
 10 omega 52.00 130.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 15.0000 -90.0000 78
 11 omega 82.00 113.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 30.0000 150.0000 31
 12 omega 41.00 69.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -30.0000 -60.0000 28
 13 omega 36.00 91.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -30.0000 -30.0000 55
 14 omega 36.00 73.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -30.0000 -150.0000 37
 15 omega 29.00 99.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -94.0000 -180.0000 70
 16 omega 49.00 75.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 -45.0000 150.0000 26
 17 omega 109.00 178.00 1.0000 2.0000
 omega____ theta____ kappa____ phi______ frames
 - 113.0000 111.0000 -150.0000 69
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1023239
_diffrn_orient_matrix_UB_12      -0.0611301
_diffrn_orient_matrix_UB_13      0.047727
_diffrn_orient_matrix_UB_21      -0.1818609
_diffrn_orient_matrix_UB_22      -0.0253452
_diffrn_orient_matrix_UB_23      0.0284815
_diffrn_orient_matrix_UB_31      -0.0387637
_diffrn_orient_matrix_UB_32      -0.0422898
_diffrn_orient_matrix_UB_33      -0.0860996
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8941
_diffrn_reflns_theta_full        76.64
_diffrn_reflns_theta_max         76.4460
_diffrn_reflns_theta_min         3.6950
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.43085
_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            colorless
_exptl_crystal_density_diffrn    1.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       solid
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         4432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.1059P)^2^+0.2969P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1529
_reflns_number_gt                3998
_reflns_number_total             4432
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol7b02574_si_002.cif
_cod_data_source_block           20150830A
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1547554