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_4126521
_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, 2(C H2 Cl2)'
_chemical_formula_sum            'C60 H86 Cl4 Ga2 N4 P12'
_chemical_formula_weight         1516.20
_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             2016-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.539(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.45280(10)
_cell_length_b                   21.4367(3)
_cell_length_c                   16.4206(3)
_cell_measurement_reflns_used    14996
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4410
_cell_measurement_theta_min      7.5660
_cell_volume                     3527.19(10)
_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      100.00(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 0.992
_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   -117.00  -2.00   1.00    6.00    --  -38.50 -19.00 120.00  115
  2  \w    -61.00  34.00   1.00    6.00    --  -38.50  38.00 -60.00   95
  3  \w      1.00  82.00   1.00    6.00    --   42.50 -99.00-180.00   81
  4  \w     30.00 109.00   1.00   24.00    --  111.00 -94.00-180.00   79
  5  \w     39.00 121.00   1.00   24.00    --  111.00-125.00-180.00   82
  6  \w     40.00 135.00   1.00   24.00    --  111.00 -45.00 -90.00   95
  7  \w     87.00 178.00   1.00   24.00    --  111.00  45.00  30.00   91
  8  \w     94.00 178.00   1.00   24.00    --  111.00 125.00-120.00   84
  9  \w     80.00 178.00   1.00   24.00    --  111.00  77.00  60.00   98
 10  \w     40.00 135.00   1.00   24.00    --  111.00 -45.00   0.00   95
 11  \w     30.00 109.00   1.00   24.00    --  111.00 -94.00-120.00   79
 12  \w     88.00 178.00   1.00   24.00    --  111.00  38.00  11.00   90
 13  \w     40.00 135.00   1.00   24.00    --  111.00 -45.00 120.00   95
 14  \w     87.00 178.00   1.00   24.00    --  111.00  30.00 -60.00   91
 15  \w     16.00  86.00   1.00    6.00    --   42.50  57.00 -30.00   70
;
_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      0.1389468000
_diffrn_orient_matrix_UB_12      0.0137374000
_diffrn_orient_matrix_UB_13      -0.0108066000
_diffrn_orient_matrix_UB_21      0.0658865000
_diffrn_orient_matrix_UB_22      -0.0321245000
_diffrn_orient_matrix_UB_23      0.0856606000
_diffrn_orient_matrix_UB_31      -0.0034798000
_diffrn_orient_matrix_UB_32      -0.0627534000
_diffrn_orient_matrix_UB_33      -0.0461741000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12085
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.595
_diffrn_reflns_theta_min         3.483
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.219
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         12085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9902
_reflns_number_total             12085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07704_si_008.cif
_cod_data_source_block           5_1
_cod_original_cell_volume        3527.19(9)
_cod_database_code               4126521
_chemical_oxdiff_formula         'C120 H172 Cl8 Ga4 N8 P24 '
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7638(14) 0.2362(14)
2. 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
3.a Ternary CH refined with riding coordinates:
 C15(H15), C27(H27), C24(H24), C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C20(H20), C21(H21), C22(H22), C10(H10), C8(H8), C9(H9)
3.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C4(H4A,H4B,H4C), C17(H17A,H17B,H17C), C28(H28A,H28B,H28C),
 C16(H16A,H16B,H16C), C29(H29A,H29B,H29C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              65375
_shelx_hkl_checksum              83127
_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 1.877
_oxdiff_exptl_absorpt_empirical_full_min 0.580
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
_twin_special_details
;
Component 2 rotated by -178.2146\% 
 around [0.00 1.00 0.01] (reciprocal) or [0.01 1.00 0.02] (direct)
;