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_4126538
_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 H82 Ga2 N4 P12, 5(C6 H6)'
_chemical_formula_sum            'C88 H112 Ga2 N4 P12'
_chemical_formula_weight         1736.89
_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
_audit_creation_date             2016-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                62.9694(19)
_cell_angle_beta                 89.6719(17)
_cell_angle_gamma                80.6194(16)
_cell_formula_units_Z            1
_cell_length_a                   10.2156(2)
_cell_length_b                   15.5486(3)
_cell_length_c                   15.9803(3)
_cell_measurement_reflns_used    14623
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.3730
_cell_measurement_theta_min      4.3980
_cell_volume                     2224.02(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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_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 0.985
_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   -111.00 -37.00   0.50    2.50    --  -38.50 -38.00-180.00  148
  2  \w    -63.00  -5.00   0.50    2.50    --  -38.50 125.00 -30.00  116
  3  \w   -116.00  -5.00   0.50    2.50    --  -38.50 -19.00-120.00  222
  4  \w      3.00  30.00   0.50    2.50    --   42.50 -99.00 150.00   54
  5  \w     30.00  97.00   0.50    2.50    --   42.50-130.00 153.00  134
  6  \w     48.00  95.00   0.50    2.50    --   42.50-139.00 -21.00   94
  7  \w     40.00  87.00   0.50   10.00    --  111.00-125.00 120.00   94
  8  \w    140.00 173.00   0.50   10.00    --  111.00  45.00 150.00   66
  9  \w     50.00 138.00   0.50   10.00    --  111.00 -61.00 -90.00  176
 10  \w     61.00 110.00   0.50   10.00    --  111.00-125.00-150.00   98
 11  \w     83.00 178.00   0.50   10.00    --  111.00  77.00  90.00  190
 12  \w     49.00  83.00   0.50   10.00    --  111.00 -61.00 150.00   68
 13  \w    134.00 174.00   0.50   10.00    --  111.00 125.00   0.00   80
 14  \w     74.00  99.00   0.50   10.00    --  111.00 -94.00   0.00   50
 15  \w     41.00 118.00   0.50   10.00    --  111.00-125.00 -90.00  154
 16  \w     93.00 123.00   0.50   10.00    --  111.00  45.00 150.00   60
 17  \w     92.00 120.00   0.50   10.00    --  111.00-125.00   0.00   56
 18  \w     44.00 128.00   0.50   10.00    --  111.00-139.00 -21.00  168
 19  \w     88.00 158.00   0.50   10.00    --  111.00  45.00-180.00  140
 20  \w     84.00 114.00   0.50   10.00    --  111.00  77.00 120.00   60
 21  \w    120.00 149.00   0.50   10.00    --  111.00  77.00 120.00   58
 22  \w    151.00 178.00   0.50   10.00    --  111.00  77.00 120.00   54
 23  \w     54.00 121.00   0.50   10.00    --  111.00-125.00  90.00  134
 24  \w     84.00 139.00   0.50   10.00    --  111.00 -77.00  30.00  110
 25  \w     88.00 153.00   0.50   10.00    --  111.00  77.00-120.00  130
 26  \w     94.00 121.00   0.50   10.00    --  111.00-125.00-180.00   54
 27  \w     96.00 177.00   0.50   10.00    --  111.00  45.00  30.00  162
 28  \w    109.00 147.00   0.50   10.00    --  111.00 125.00-180.00   76
 29  \w    137.00 141.50   0.50   10.00    --  111.00 125.00  30.00    9
;
_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      0.0328780000
_diffrn_orient_matrix_UB_12      -0.0448807000
_diffrn_orient_matrix_UB_13      0.1070944000
_diffrn_orient_matrix_UB_21      -0.1392432000
_diffrn_orient_matrix_UB_22      -0.0277504000
_diffrn_orient_matrix_UB_23      0.0173913000
_diffrn_orient_matrix_UB_31      0.0550938000
_diffrn_orient_matrix_UB_32      -0.1000129000
_diffrn_orient_matrix_UB_33      0.0035369000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21299
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.496
_diffrn_reflns_theta_min         3.114
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.130
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       needle
_exptl_crystal_F_000             910
_exptl_crystal_size_max          0.488
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.441
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         9205
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0750P)^2^+1.5961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1279
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8652
_reflns_number_total             9205
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07704_si_009.cif
_cod_data_source_block           5_2
_cod_original_cell_volume        2224.01(8)
_cod_database_code               4126538
_chemical_oxdiff_formula         'C88 H112 Ga2 N4 P12 '
_reflns_odcompleteness_completeness 99.99
_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.a Ternary CH refined with riding coordinates:
 C24(H24), C15(H15), C27(H27), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C21(H21), C22(H22), C20(H20), C10(H10), C9(H9), C42(H42),
 C44(H44), C30(H30), C31(H31), C40(H40), C43(H43), C39(H39), C35(H35), C32(H32),
  C34(H34), C33(H33), C41(H41), C38(H38), C37(H37), C36(H36)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C),
 C28(H28A,H28B,H28C), C13(H13A,H13B,H13C), C16(H16A,H16B,H16C), C29(H29A,H29B,
 H29C), C25(H25A,H25B,H25C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              69108
_shelx_hkl_checksum              42806
_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 1.419
_oxdiff_exptl_absorpt_empirical_full_min 0.493