Ruthenium mediated halogenation of white phosphorus: synthesis and reactivity of the unprecedented P<sub>4</sub>Cl<sub>2</sub> moiety.
Bispinghoff, Mark; Benkő, Zoltán; Grützmacher, Hansjörg; Calvo, Fuencisla Delgado; Caporali, Maria; Peruzzini, Maurizio; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3593–3600; doi:10.1039/c8dt01840e

data_7047956
_publ_section_title
;
 Ruthenium mediated halogenation of white phosphorus: synthesis and
 reactivity of the unprecedented P<sub>4</sub>Cl<sub>2</sub> moiety.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3593
_journal_page_last               3600
_journal_paper_doi               10.1039/c8dt01840e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C56 H96 P8 Ru4, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H112 O2 P8 Ru4'
_chemical_formula_weight         1565.57
_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     dual
_audit_creation_date             2016-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2018-01-05 deposited with the CCDC.
2018-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                112.290(2)
_cell_angle_beta                 107.073(2)
_cell_angle_gamma                90.803(2)
_cell_formula_units_Z            1
_cell_length_a                   11.9212(3)
_cell_length_b                   12.4576(3)
_cell_length_c                   13.0288(3)
_cell_measurement_reflns_used    9724
_cell_measurement_temperature    104(2)
_cell_measurement_theta_max      32.1380
_cell_measurement_theta_min      3.2730
_cell_volume                     1694.14(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      104(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -40.00  43.00   1.00   50.00    --   26.86 -57.00 -60.00   83
  2  \w     20.00  69.00   1.00   50.00    --   26.86 -99.00  60.00   49
  3  \w      8.00  94.00   1.00   50.00    --   26.86  57.00-180.00   86
  4  \w     -9.00  69.00   1.00   50.00    --   26.86 -99.00 -90.00   78
  5  \w     42.00  69.00   1.00   50.00    --   26.86 -99.00-180.00   27
  6  \w    -16.00 100.00   1.00   50.00    --   26.86  19.00 120.00  116
  7  \w    -52.00 -25.00   1.00   50.00    --  -26.23  38.00  90.00   27
  8  \w    -42.00  48.00   1.00   50.00    --   26.86 -57.00 150.00   90
  9  \w      6.00  96.00   1.00   50.00    --   26.86  57.00 -60.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0377832000
_diffrn_orient_matrix_UB_12      -0.0536278000
_diffrn_orient_matrix_UB_13      -0.0376701000
_diffrn_orient_matrix_UB_21      0.0278729000
_diffrn_orient_matrix_UB_22      -0.0067478000
_diffrn_orient_matrix_UB_23      -0.0428404000
_diffrn_orient_matrix_UB_31      0.0418215000
_diffrn_orient_matrix_UB_32      -0.0307043000
_diffrn_orient_matrix_UB_33      0.0247184000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22671
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.872
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.894
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         8394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0300P)^2^+1.7334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6964
_reflns_number_total             8394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01840e2.cif
_cod_data_source_block           mb175smart
_cod_depositor_comments
'Adding full bibliography for 7047955--7047958.cif.'
_cod_database_code               7047956
_chemical_oxdiff_formula         C32H56OP4Ru2
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21a,H21b), C25(H25a,H25b), C26(H26a,H26b), C22(H22a,H22b), C23(H23a,
 H23b), C27(H27a,H27b), C31(H31a,H31b), C32(H32a,H32b), C29(H29a,H29b),
 C30(H30a,H30b)
2.b Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C17(H17a,H17b,H17c), C16(H16a,H16b,H16c),
 C18(H18a,H18b,H18c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c), C19(H19a,H19b,H19c),
 C20(H20a,H20b,H20c), C10(H10a,H10b,H10c), C28(H28a,H28b,H28c), C24(H24a,H24b,
 H24c)
;
_shelx_res_checksum              82502
_shelx_shelxl_version_number     2014/7
_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 1.064
_oxdiff_exptl_absorpt_empirical_full_min 0.973