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_7047955
_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         'C38 H63 Cl P5 Ru2, Cl4 Ga, C4 H10 O2'
_chemical_formula_sum            'C42 H73 Cl5 Ga O2 P5 Ru2'
_chemical_formula_weight         1213.96
_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     dual
_audit_creation_date             2016-11-01
_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                90
_cell_angle_beta                 94.033(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5596(3)
_cell_length_b                   32.7266(13)
_cell_length_c                   16.3335(5)
_cell_measurement_reflns_used    4240
_cell_measurement_temperature    106.5(6)
_cell_measurement_theta_max      27.4710
_cell_measurement_theta_min      2.8340
_cell_volume                     5097.3(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_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      106.5(6)
_diffrn_detector                 'Oxford Diffraction Sapphire 3'
_diffrn_detector_area_resol_mean 8.26
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_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    -47.00  46.00   1.00  120.00    --  -21.63  38.00  30.00   93
  2  \w    -19.00   8.00   1.00  120.00    --  -21.63 -99.00 -90.00   27
  3  \w    -40.00   6.00   1.00  120.00    --  -21.63  19.00 -60.00   46
  4  \w     23.00  49.00   1.00  120.00    --  -21.63  19.00 -60.00   26
  5  \w     42.00  94.00   1.00  120.00    --   22.10 179.00 -90.00   52
  6  \w    -94.00 -83.00   1.00  120.00    --  -21.63 -38.00-150.00   11
;
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0340141000
_diffrn_orient_matrix_UB_12      0.0134416000
_diffrn_orient_matrix_UB_13      0.0290681000
_diffrn_orient_matrix_UB_21      0.0052737000
_diffrn_orient_matrix_UB_22      0.0149298000
_diffrn_orient_matrix_UB_23      -0.0311056000
_diffrn_orient_matrix_UB_31      -0.0659588000
_diffrn_orient_matrix_UB_32      0.0081343000
_diffrn_orient_matrix_UB_33      0.0090445000
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.1060
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24113
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.786
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.563
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99398
_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 brown'
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         10407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0332P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6914
_reflns_number_total             10407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01840e2.cif
_cod_data_source_block           mb207r-x1smart
_cod_depositor_comments
'Adding full bibliography for 7047955--7047958.cif.'
_cod_database_code               7047955
_chemical_oxdiff_formula         'C50 H100 Ru2 P5 Cl5 Ga O2'
_chemical_oxdiff_usercomment     'frame 5 appended after user stop'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C33(H33), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34a,H34b), C28(H28a,H28b), C22(H22a,H22b), C38(H38a,H38b), C32(H32a,
 H32b), C31(H31a,H31b), C37(H37a,H37b), C23(H23a,H23b), C26(H26a,H26b),
 C36(H36a,H36b), C35(H35a,H35b), C30(H30a,H30b), C25(H25a,H25b), C29(H29a,H29b),
  C24(H24a,H24b), C40(H40a,H40b), C41(H41a,H41b)
2.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C10(H10a,H10b,H10c), C6(H6a,H6b,H6c), C7(H7a,H7b,H7c),
 C9(H9a,H9b,H9c), C19(H19a,H19b,H19c), C17(H17a,H17b,H17c), C20(H20a,H20b,H20c),
  C16(H16a,H16b,H16c), C18(H18a,H18b,H18c), C42(H42a,H42b,H42c), C39(H39a,H39b,
 H39c)
;
_shelx_res_checksum              21871
_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 1.029
_oxdiff_exptl_absorpt_empirical_full_min 0.982