Selective Derivatization of a Hexaphosphane from Functionalization of White Phosphorus.
Hennersdorf, Felix; Frötschel, Julia; Weigand, Jan J.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07704

data_4126537
_publ_section_title
;
 Selective Derivatization of a Hexaphosphane from Functionalization of
 White Phosphorus.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07704
_journal_year                    2017
_chemical_formula_moiety         'C58 H83 Cl Ga2 N4 P6, 2(C6 H5 F)'
_chemical_formula_sum            'C70 H93 Cl F2 Ga2 N4 P6'
_chemical_formula_weight         1389.19
_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
_audit_creation_date             2016-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                89.9560(12)
_cell_angle_beta                 68.6852(13)
_cell_angle_gamma                89.3864(11)
_cell_formula_units_Z            2
_cell_length_a                   13.31652(16)
_cell_length_b                   15.5916(2)
_cell_length_c                   18.1014(3)
_cell_measurement_reflns_used    30069
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      76.3260
_cell_measurement_theta_min      4.5370
_cell_volume                     3501.02(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_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   -108.00 -12.00   0.50    2.00    --  -38.50 -57.00  90.00  192
  2  \w    -38.00   0.00   0.50    2.00    --  -38.50  38.00 -60.00   76
  3  \w    -52.00  34.00   0.50    2.00    --  -38.50  38.00-120.00  172
  4  \w    -37.00  -7.00   0.50    2.00    --  -38.50 125.00 -60.00   60
  5  \w     33.00  62.00   0.50    2.00    --   42.75 -57.00-180.00   58
  6  \w    -27.00  29.00   0.50    2.00    --   42.75 -77.00 -30.00  112
  7  \w     24.00  96.00   0.50    2.00    --   42.75-125.00  60.00  144
  8  \w    120.00 174.00   0.50    8.00    --  111.00  15.00 150.00  108
  9  \w     72.00 109.00   0.50    8.00    --  111.00 -94.00  30.00   74
 10  \w    136.00 169.00   0.50    8.00    --  111.00  45.00-150.00   66
 11  \w     58.00 120.00   0.50    8.00    --  111.00 -61.00   0.00  124
 12  \w     68.00 132.00   0.50    8.00    --  111.00 -30.00-180.00  128
 13  \w     43.00 121.00   0.50    8.00    --  111.00-125.00  30.00  156
 14  \w    121.00 173.00   0.50    8.00    --  111.00  45.00-180.00  104
 15  \w     96.00 121.00   0.50    8.00    --  111.00-125.00-120.00   50
 16  \w     52.00  87.00   0.50    8.00    --  111.00-125.00-120.00   70
 17  \w     45.00 114.00   0.50    8.00    --  111.00 -61.00-150.00  138
 18  \w     37.00 104.00   0.50    8.00    --  111.00 -30.00   0.00  134
 19  \w     89.00 121.00   0.50    8.00    --  111.00-125.00 150.00   64
 20  \w     48.00  95.00   0.50    8.00    --  111.00-125.00   0.00   94
 21  \w     31.00 108.00   0.50    8.00    --  111.00 -94.00-180.00  154
 22  \w     56.00  95.00   0.50    8.00    --  111.00 -94.00-120.00   78
 23  \w     55.00  82.00   0.50    8.00    --  111.00 -77.00 120.00   54
 24  \w    103.00 129.00   0.50    8.00    --  111.00 -77.00 120.00   52
 25  \w     39.00  71.00   0.50    8.00    --  111.00-125.00 -30.00   64
 26  \w     91.00 121.00   0.50    8.00    --  111.00-125.00 -30.00   60
 27  \w     39.00  90.00   0.50    8.00    --  111.00-125.00  60.00  102
 28  \w    102.00 177.00   0.50    8.00    --  111.00 125.00-120.00  150
 29  \w     89.00 173.00   0.50    8.00    --  111.00  45.00-120.00  168
 30  \w     95.00 128.00   0.50    8.00    --  111.00 125.00 -60.00   66
 31  \w    122.00 148.00   0.50    8.00    --  111.00 125.00-180.00   52
 32  \w     99.00 175.00   0.50    8.00    --  111.00 125.00 -90.00  152
 33  \w     88.00 124.00   0.50    8.00    --  111.00  45.00-150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0062608000
_diffrn_orient_matrix_UB_12      -0.0898017000
_diffrn_orient_matrix_UB_13      -0.0333989000
_diffrn_orient_matrix_UB_21      -0.1214685000
_diffrn_orient_matrix_UB_22      0.0137848000
_diffrn_orient_matrix_UB_23      0.0185339000
_diffrn_orient_matrix_UB_31      0.0250879000
_diffrn_orient_matrix_UB_32      0.0388544000
_diffrn_orient_matrix_UB_33      -0.0829886000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0191
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            37546
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.609
_diffrn_reflns_theta_min         2.620
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.967
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       plate
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.388
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         14543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.290
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.2565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1088
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14516
_reflns_number_total             14543
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07704_si_023.cif
_cod_data_source_block           10_2
_cod_original_cell_volume        3501.03(9)
_cod_database_code               4126537
_chemical_oxdiff_formula         C70H93ClF2Ga2N4P6
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl1B)=Sof(P1B)=Sof(P2B)=Sof(P3B)=Sof(P4B)=Sof(H4E)=Sof(P5B)=Sof(P6B)=1-
 FVAR(1)
 Sof(Cl1A)=Sof(P1A)=Sof(P2A)=Sof(P3A)=Sof(P4A)=Sof(H4D)=Sof(P5A)=Sof(P6A)=
 FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C41(H41), C44(H44), C53(H53), C56(H56)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31),
 C37(H37), C38(H38), C39(H39), C49(H49), C50(H50), C51(H51), C60(H60), C61(H61),
  C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              88782
_shelx_hkl_checksum              62758
_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 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.611