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_4126530
_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 P4'
_chemical_formula_sum            'C58 H82 Ga2 N4 P4'
_chemical_formula_weight         1098.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7471(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.34458(19)
_cell_length_b                   18.10118(18)
_cell_length_c                   43.7739(4)
_cell_measurement_reflns_used    45624
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4640
_cell_measurement_theta_min      3.4120
_cell_volume                     14518.8(2)
_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      100.01(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 0.986
_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    -61.00  34.00   0.50    1.50    --  -38.50  38.00 -90.00  190
  2  \w     23.00  98.00   0.50    1.50    --   42.50-125.00-180.00  150
  3  \w     23.00  98.00   0.50    1.50    --   42.50-125.00  60.00  150
  4  \w     23.00  98.00   0.50    1.50    --   42.50-125.00 -60.00  150
  5  \w     16.00 113.00   0.50    1.50    --   42.50  57.00-180.00  194
  6  \w     23.00  98.00   0.50    1.50    --   42.50-125.00   0.00  150
  7  \w     87.00 178.00   0.50    6.00    --  111.00  30.00 150.00  182
  8  \w     37.00 142.00   0.50    6.00    --  111.00 -77.00 -90.00  210
  9  \w     30.00 109.00   0.50    6.00    --  111.00 -94.00  60.00  158
 10  \w     31.00 156.00   0.50    6.00    --  111.00 -15.00-120.00  250
 11  \w     40.00 135.00   0.50    6.00    --  111.00 -45.00-120.00  190
 12  \w     30.00 109.00   0.50    6.00    --  111.00 -94.00-150.00  158
 13  \w     30.00 109.00   0.50    6.00    --  111.00 -94.00  90.00  158
 14  \w     87.00 178.00   0.50    6.00    --  111.00  30.00 120.00  182
 15  \w     80.00 178.00   0.50    6.00    --  111.00  77.00  30.00  196
 16  \w     11.00 116.00   0.50    1.50    --   42.50  77.00 -60.00  210
 17  \w     16.00 113.00   0.50    1.50    --   42.50  57.00 -90.00  194
 18  \w     16.00 113.00   0.50    1.50    --   42.50  57.00   0.00  194
 19  \w     11.00 116.00   0.50    1.50    --   42.50  77.00  60.00  210
 20  \w     66.00 140.00   0.50    6.00    --  111.00  15.00 -30.00  148
;
_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      -0.0574751000
_diffrn_orient_matrix_UB_12      0.0219060000
_diffrn_orient_matrix_UB_13      0.0229327000
_diffrn_orient_matrix_UB_21      -0.0555750000
_diffrn_orient_matrix_UB_22      -0.0523901000
_diffrn_orient_matrix_UB_23      -0.0161903000
_diffrn_orient_matrix_UB_31      0.0261885000
_diffrn_orient_matrix_UB_32      -0.0633734000
_diffrn_orient_matrix_UB_33      0.0212630000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            77051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.807
_diffrn_reflns_theta_min         3.432
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.976
_exptl_absorpt_correction_T_max  0.547
_exptl_absorpt_correction_T_min  0.261
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.005
_exptl_crystal_description       block
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.184
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         15110
_refine_ls_number_restraints     396
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0471P)^2^+33.7644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14348
_reflns_number_total             15110
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07704_si_004.cif
_cod_data_source_block           2_2
_cod_database_code               4126530
_chemical_oxdiff_formula         'C512 H648 Cl57 Ga16 N32 P32 '
_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. Uiso/Uaniso restraints and constraints
N2A \\sim C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim
C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim N2B \\sim
C18B \\sim C19B \\sim C20B \\sim C21B \\sim C22B \\sim C23B \\sim C24B \\sim
C25B \\sim C26B \\sim C27B \\sim C28B \\sim C29B: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
3. Others
 Sof(N2B)=Sof(C18B)=Sof(C19B)=Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25D)=
 Sof(H25E)=Sof(H25F)=Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27B)=
 Sof(H27B)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(N2A)=Sof(C18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27A)=
 Sof(H27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24A(H24A), C27A(H27A), C41(H41), C44(H44), C53(H53),
 C56(H56), C24B(H24B), C27B(H27B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C9(H9), C10(H10), C20A(H20A), C21A(H21A), C22A(H22A),
 C31(H31), C37(H37), C38(H38), C39(H39), C49(H49), C50(H50), C51(H51),
 C20B(H20B), C21B(H21B), C22B(H22B)
4.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), C25A(H25A,H25B,H25C), C26A(H26A,H26B,
 H26C), C28A(H28A,H28B,H28C), C29A(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), C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F),
 C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F)
;
_shelx_res_checksum              90183
_shelx_hkl_checksum              14693
_shelx_fab_checksum              90007
_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 1.620
_oxdiff_exptl_absorpt_empirical_full_min 0.561