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_4126526
_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, 3(C H2 Cl2)'
_chemical_formula_sum            'C61 H88 Cl6 Ga2 N4 P4'
_chemical_formula_weight         1353.37
_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             2017-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7064(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8363(4)
_cell_length_b                   39.5996(9)
_cell_length_c                   18.2132(4)
_cell_measurement_reflns_used    21578
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1910
_cell_measurement_theta_min      2.5970
_cell_volume                     13557.0(5)
_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 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.951
_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    -70.00  35.00   0.50    6.00    --  -38.50  77.00 120.00  210
  2  \w     11.00  69.00   0.50    6.00    --   42.50 -57.00-120.00  116
  3  \w     41.00 111.00   0.50    6.00    --   42.50  38.00 -90.00  140
  4  \w    118.00 162.00   0.50   24.00    --  111.00 125.00-120.00   88
  5  \w     84.00 139.00   0.50   24.00    --  111.00 -77.00 150.00  110
  6  \w     84.00 176.00   0.50   24.00    --  111.00  61.00 -60.00  184
  7  \w     88.00 177.00   0.50   24.00    --  111.00  30.00  90.00  178
  8  \w    102.00 167.00   0.50   24.00    --  111.00  30.00  30.00  130
  9  \w     66.00 118.00   0.50   24.00    --  111.00-125.00   0.00  104
 10  \w     93.00 121.00   0.50   24.00    --  111.00-125.00 120.00   56
 11  \w     30.00 107.00   0.50   24.00    --  111.00 -94.00   0.00  154
 12  \w     53.00 116.00   0.50   24.00    --  111.00-137.00-161.00  126
;
_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      -0.0325633000
_diffrn_orient_matrix_UB_12      -0.0248831000
_diffrn_orient_matrix_UB_13      -0.0576102000
_diffrn_orient_matrix_UB_21      0.0254261000
_diffrn_orient_matrix_UB_22      -0.0298908000
_diffrn_orient_matrix_UB_23      0.0491978000
_diffrn_orient_matrix_UB_31      -0.0707662000
_diffrn_orient_matrix_UB_32      0.0007899000
_diffrn_orient_matrix_UB_33      0.0380508000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66262
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.386
_diffrn_reflns_theta_min         2.351
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.342
_exptl_absorpt_correction_T_max  0.702
_exptl_absorpt_correction_T_min  0.587
_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    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             5648
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1427
_refine_ls_number_reflns         27376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0735
_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^)+(0.1081P)^2^+16.9981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2035
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19589
_reflns_number_total             27376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07704_si_005.cif
_cod_data_source_block           2_3
_cod_database_code               4126526
_chemical_oxdiff_formula         C61H88Cl6Ga2N4P4
_reflns_odcompleteness_completeness 98.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2.a Ternary CH refined with riding coordinates:
 C12A(H12A), C15A(H15A), C24A(H24A), C27A(H27A), C41A(H41A), C44A(H44A),
 C53A(H53A), C56A(H56A), C12B(H12B), C15B(H15B), C24B(H24B), C27B(H27B),
 C41B(H41B), C44B(H44B), C53B(H53B), C56B(H56B)
2.b Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C63(H63A,H63B), C62(H62A,H62B), C59(H59A,H59B), C60(H60A,
 H60B), C64(H64A,H64B)
2.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C8A(H8A), C9A(H9A), C10A(H10A), C20A(H20A), C21A(H21A), C22A(H22A),
 C31A(H31A), C37A(H37A), C38A(H38A), C39A(H39A), C49A(H49A), C50A(H50A),
 C51A(H51A), C2B(H2B), C8B(H8B), C9B(H9B), C10B(H10B), C20B(H20B), C21B(H21B),
 C22B(H22B), C31B(H31B), C37B(H37B), C38B(H38B), C39B(H39B), C49B(H49B),
 C50B(H50B), C51B(H51B)
2.d Idealised Me refined as rotating group:
 C4A(H4AA,H4AB,H4AC), C5A(H5AA,H5AB,H5AC), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C25A(H25A,H25B,H25C),
 C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C33A(H33A,
 H33B,H33C), C34A(H34A,H34B,H34C), C42A(H42A,H42B,H42C), C43A(H43A,H43B,H43C),
 C45A(H45A,H45B,H45C), C46A(H46A,H46B,H46C), C54A(H54A,H54B,H54C), C55A(H55A,
 H55B,H55C), C57A(H57A,H57B,H57C), C58A(H58A,H58B,H58C), C4B(H4BA,H4BB,H4BC),
 C5B(H5BA,H5BB,H5BC), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C16B(H16D,
 H16E,H16F), C17B(H17D,H17E,H17F), C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F),
 C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C33B(H33D,H33E,H33F), C34B(H34D,
 H34E,H34F), C42B(H42D,H42E,H42F), C43B(H43D,H43E,H43F), C45B(H45D,H45E,H45F),
 C46B(H46D,H46E,H46F), C54B(H54D,H54E,H54F), C55B(H55D,H55E,H55F), C57B(H57D,
 H57E,H57F), C58B(H58D,H58E,H58F)
;
_shelx_res_checksum              61105
_shelx_hkl_checksum              36982
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 4.673
_oxdiff_exptl_absorpt_empirical_full_min 0.317