Direct Functionalization of White Phosphorus to Cyclotetraphosphanes: Selective Formation of Four P-C Bonds.
Du, Shanshan; Yang, Jimin; Hu, Jingyuan; Chai, Zhengqi; Luo, Gen; Luo, Yi; Zhang, Wen-Xiong; Xi, Zhenfeng; Journal of the American Chemical Society 141 (2019) 6843–6847; doi:10.1021/jacs.9b02628

data_4128136
_publ_section_title
;
 Direct Functionalization of White Phosphorus to Cyclotetraphosphanes:
 Selective Formation of Four P-C Bonds.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6843
_journal_page_last               6847
_journal_paper_doi               10.1021/jacs.9b02628
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C34 H74 Al2 P4 Si4'
_chemical_formula_sum            'C34 H74 Al2 P4 Si4'
_chemical_formula_weight         773.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9811(2)
_cell_length_b                   16.4506(3)
_cell_length_c                   17.9869(3)
_cell_measurement_reflns_used    25952
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.8060
_cell_measurement_theta_min      3.6230
_cell_volume                     4432.84(12)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -33.00  30.00   0.50    6.00    --   -9.50 -82.00 -90.00  126
  2  \w    -98.00  28.00   0.50    6.00    --   -9.50 -38.00 -90.00  252
  3  \w     -8.00  18.00   0.50    6.00    --   -9.50 -82.00  60.00   52
  4  \w    -80.00  78.00   0.50    6.00    --   -9.50  19.00 -90.00  316
  5  \w    -82.00 -56.00   0.50    6.00    --   -9.50 -19.00-150.00   52
  6  \w     12.00  60.00   0.50    6.00    --   -9.50 -19.00-150.00   96
  7  \w    -12.00  13.00   0.50    6.00    --   -9.50 -57.00 -30.00   50
  8  \w    -82.00  20.00   0.50    6.00    --   -9.50 -57.00  60.00  204
  9  \w    -46.00  24.00   0.50    6.00    --   -9.50  38.00 -90.00  140
 10  \w      7.00  32.00   0.50    6.00    --    9.80  57.00 120.00   50
 11  \w     60.00  85.00   0.50    6.00    --    9.80  57.00 120.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0334341000
_diffrn_orient_matrix_UB_12      -0.0109845000
_diffrn_orient_matrix_UB_13      0.0260354000
_diffrn_orient_matrix_UB_21      0.0334927000
_diffrn_orient_matrix_UB_22      -0.0108499000
_diffrn_orient_matrix_UB_23      0.0260505000
_diffrn_orient_matrix_UB_31      -0.0001079000
_diffrn_orient_matrix_UB_32      0.0402545000
_diffrn_orient_matrix_UB_33      0.0141515000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            78841
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.54
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86874
_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            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.708
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.41(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     430
_refine_ls_number_reflns         8681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0779
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1390P)^2^+8.4830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2042
_refine_ls_wR_factor_ref         0.2104
_reflns_number_gt                8015
_reflns_number_total             8681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9b02628_si_002.cif
_cod_data_source_block           3
_cod_database_code               4128136
_chemical_oxdiff_formula         'C1 H1 Si1 P1 Al1'
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H32c)=Sof(H32d)=Sof(C33A)=Sof(H33d)=Sof(H33e)=Sof(H33f)=1-FVAR(1)
 Sof(H32a)=Sof(H32b)=Sof(C33)=Sof(H33a)=Sof(H33b)=Sof(H33c)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13a,H13b), C15(H15a,H15b), C30(H30a,H30b), C32(H32a,H32b), C32(H32c,H32d)
3.b Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,
 H9b,H9c), C10(H10a,H10b,H10c), C11(H11a,H11b,H11c), C12(H12a,H12b,H12c),
 C14(H14a,H14b,H14c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C22(H22a,H22b,
 H22c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C25(H25a,H25b,H25c), C26(H26a,
 H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c), C29(H29a,H29b,H29c),
 C31(H31a,H31b,H31c), C33(H33a,H33b,H33c), C33A(H33d,H33e,H33f), C34(H34a,H34b,
 H34c)
;
_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 1.258
_oxdiff_exptl_absorpt_empirical_full_min 0.843