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_4126539
_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         'C60 H85 F3 Ga2 N4 O3 P6 S'
_chemical_formula_sum            'C60 H85 F3 Ga2 N4 O3 P6 S'
_chemical_formula_weight         1324.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-05-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.9790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.95819(19)
_cell_length_b                   17.83215(13)
_cell_length_c                   17.44947(15)
_cell_measurement_reflns_used    26849
_cell_measurement_temperature    100.00(16)
_cell_measurement_theta_max      76.5540
_cell_measurement_theta_min      3.2480
_cell_volume                     6421.35(10)
_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      100.00(16)
_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    -98.00 -47.00   0.50    1.00    --  -38.50 134.00 156.00  102
  2  \w    -93.00 -66.00   0.50    1.00    --  -38.50 125.00  90.00   54
  3  \w   -111.00 -16.00   0.50    1.00    --  -38.50 -38.00 -90.00  190
  4  \w   -106.00 -14.00   0.50    1.00    --  -38.50 -57.00-180.00  184
  5  \w     78.00 126.00   0.50    3.00    --  111.00 -61.00   0.00   96
  6  \w     72.00 135.00   0.50    3.00    --  111.00 -45.00 -30.00  126
  7  \w    127.00 177.00   0.50    3.00    --  111.00  61.00 -60.00  100
  8  \w    143.00 177.00   0.50    3.00    --  111.00  61.00 -30.00   68
  9  \w    115.00 177.00   0.50    3.00    --  111.00  61.00  90.00  124
 10  \w     85.00 118.00   0.50    3.00    --  111.00 -45.00 120.00   66
 11  \w     90.00 120.00   0.50    3.00    --  111.00-125.00 120.00   60
 12  \w     54.00 103.00   0.50    3.00    --  111.00 -94.00  30.00   98
 13  \w     49.00 131.00   0.50    3.00    --  111.00 -30.00 150.00  164
 14  \w     83.00 122.00   0.50    3.00    --  111.00  61.00 -30.00   78
 15  \w     40.00  67.00   0.50    3.00    --  111.00 -45.00 -30.00   54
 16  \w     39.00  96.00   0.50    3.00    --  111.00-125.00  30.00  114
 17  \w     41.00 139.00   0.50    3.00    --  111.00 -61.00 150.00  196
;
_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      -0.0400847000
_diffrn_orient_matrix_UB_12      0.0201803000
_diffrn_orient_matrix_UB_13      0.0543369000
_diffrn_orient_matrix_UB_21      0.0629825000
_diffrn_orient_matrix_UB_22      0.0136061000
_diffrn_orient_matrix_UB_23      0.0723936000
_diffrn_orient_matrix_UB_31      -0.0005916000
_diffrn_orient_matrix_UB_32      0.0829000000
_diffrn_orient_matrix_UB_33      -0.0250758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37012
_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         76.918
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.188
_exptl_absorpt_correction_T_max  0.721
_exptl_absorpt_correction_T_min  0.577
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         13385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+1.8775P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12909
_reflns_number_total             13385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07704_si_027.cif
_cod_data_source_block           14
_cod_original_cell_volume        6421.34(10)
_cod_database_code               4126539
_chemical_oxdiff_formula         'C60 H85 F3 Ga2 N4 O3 P6 S1'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C12(H12), C15(H15), C24(H24), C27(H27), C41(H41), C44(H44), C53(H53), C56(H56)
2.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)
2.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), C59(H59A,H59B,H59C)
;
_shelx_res_checksum              62559
_shelx_hkl_checksum              88466
_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 2.209
_oxdiff_exptl_absorpt_empirical_full_min 0.683