Controlled scrambling reactions to polyphosphanes via bond metathesis reactions
Schoemaker, Robin; Schwedtmann, Kai; Franconetti, Antonio; Frontera, Antonio; Hennersdorf, Felix; Weigand, Jan J.; Chemical Science  (2019) –; doi:10.1039/C9SC04501E

data_1552475
_publ_section_title
;
 Controlled scrambling reactions to polyphosphanes via bond metathesis
 reactions
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC04501E
_journal_year                    2019
_chemical_formula_moiety         'C31 H48 N P3 S'
_chemical_formula_sum            'C31 H48 N P3 S'
_chemical_formula_weight         559.67
_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             2017-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-08-30 deposited with the CCDC.    2019-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                104.8628(12)
_cell_angle_beta                 100.6013(12)
_cell_angle_gamma                90.2605(12)
_cell_formula_units_Z            8
_cell_length_a                   16.0052(2)
_cell_length_b                   17.2802(2)
_cell_length_c                   23.3958(3)
_cell_measurement_reflns_used    33640
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.4320
_cell_measurement_theta_min      2.8200
_cell_volume                     6138.29(14)
_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(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 0.989
_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    -64.00  31.00   0.50    3.00    --  -38.50  57.00  90.00  190
  2  \w   -109.00 -12.00   0.50    3.00    --  -38.50 -57.00 -60.00  194
  3  \w     32.00  74.00   0.50    3.00    --   42.75-125.00 -30.00   84
  4  \w     11.00  96.00   0.50    3.00    --   42.75  77.00-150.00  170
  5  \w     49.00  83.00   0.50    3.00    --   42.75 -99.00  90.00   68
  6  \w    -27.00  12.00   0.50    3.00    --   42.75 -77.00-180.00   78
  7  \w     87.00 135.00   0.50   12.00    --  111.00 -30.00-150.00   96
  8  \w     75.00 138.00   0.50   12.00    --  111.00 -61.00-150.00  126
  9  \w     84.00 109.00   0.50   12.00    --  111.00 -94.00-150.00   50
 10  \w     40.00 121.00   0.50   12.00    --  111.00-125.00-150.00  162
 11  \w    109.00 144.00   0.50   12.00    --  111.00 125.00 -30.00   70
 12  \w     40.00  67.00   0.50   12.00    --  111.00 -30.00-150.00   54
 13  \w    102.00 142.00   0.50   12.00    --  111.00 -77.00-120.00   80
 14  \w     41.00 121.00   0.50   12.00    --  111.00-125.00 150.00  160
 15  \w     84.00 125.00   0.50   12.00    --  111.00 -30.00  30.00   82
 16  \w     36.00  69.00   0.50   12.00    --  111.00 -30.00  30.00   66
 17  \w    123.00 150.00   0.50   12.00    --  111.00 125.00  60.00   54
 18  \w     96.00 178.00   0.50   12.00    --  111.00  30.00  30.00  164
 19  \w     91.00 121.00   0.50   12.00    --  111.00-125.00  30.00   60
 20  \w     44.00  72.00   0.50   12.00    --  111.00-125.00 -30.00   56
 21  \w     41.00  66.00   0.50   12.00    --  111.00-125.00 -60.00   50
 22  \w    101.00 144.00   0.50   12.00    --  111.00 125.00-180.00   86
 23  \w     48.00  78.00   0.50   12.00    --  111.00-125.00  30.00   60
 24  \w     56.00  83.00   0.50   12.00    --  111.00 -77.00  30.00   54
 25  \w    102.00 130.00   0.50   12.00    --  111.00 -77.00  30.00   56
 26  \w     37.00  81.00   0.50   12.00    --  111.00 -77.00-120.00   88
 27  \w    106.00 133.00   0.50   12.00    --  111.00 -61.00  30.00   54
 28  \w     45.00 121.00   0.50   12.00    --  111.00-125.00 -90.00  152
 29  \w     55.00 121.00   0.50   12.00    --  111.00-125.00  60.00  132
 30  \w     62.00  96.00   0.50   12.00    --  111.00 -94.00-180.00   68
 31  \w     73.00  98.00   0.50   12.00    --  111.00 -94.00  30.00   50
 32  \w     89.00 120.00   0.50   12.00    --  111.00-125.00 -30.00   62
 33  \w     32.00  98.00   0.50   12.00    --  111.00 -94.00  60.00  132
 34  \w     46.00 105.00   0.50   12.00    --  111.00 -94.00  90.00  118
 35  \w     30.00  74.00   0.50   12.00    --  111.00 -94.00-150.00   88
 36  \w     35.00 174.00   0.50   12.00    --  111.00   0.00-180.00  278
;
_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      -0.0726996000
_diffrn_orient_matrix_UB_12      0.0371269000
_diffrn_orient_matrix_UB_13      0.0310888000
_diffrn_orient_matrix_UB_21      0.0478882000
_diffrn_orient_matrix_UB_22      -0.0122591000
_diffrn_orient_matrix_UB_23      0.0601997000
_diffrn_orient_matrix_UB_31      0.0451596000
_diffrn_orient_matrix_UB_32      0.0836925000
_diffrn_orient_matrix_UB_33      0.0150850000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72032
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.778
_diffrn_reflns_theta_min         1.991
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_description       plate
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.039
_refine_diff_density_max         0.471
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1380
_refine_ls_number_reflns         25591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+1.7679P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0858
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21917
_reflns_number_total             25591
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           9b
_cod_original_cell_volume        6138.29(16)
_cod_database_code               1552475
_chemical_oxdiff_formula         'C248 H384 N8 P24 S8 '
_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, All C(H,H) groups, All C(H,H,H,H) groups
2. Others
 Sof(C7E)=Sof(H0)=Sof(H01Q)=Sof(H01R)=Sof(C9E)=Sof(H2A)=Sof(H2B)=Sof(C10E)=
 Sof(H3A)=Sof(H3B)=Sof(C11E)=Sof(H8AA)=Sof(H8AB)=Sof(C12E)=Sof(H4A)=Sof(H4B)=1-
 FVAR(1)
 Sof(C7D)=Sof(H8)=Sof(H01N)=Sof(H01P)=Sof(C9D)=Sof(H7A)=Sof(H7B)=Sof(C10D)=
 Sof(H6A)=Sof(H6B)=Sof(C11D)=Sof(H1A)=Sof(H1B)=Sof(C12D)=Sof(H5A)=Sof(H5B)=
 FVAR(1)
 Sof(H0GA)=Sof(C8C)=Sof(H5AA)=Sof(H5AB)=Sof(C9C)=Sof(H0AA)=Sof(H0AB)=Sof(C10C)=
 Sof(H7AA)=Sof(H7AB)=Sof(C11C)=Sof(H6AA)=Sof(H6AB)=Sof(H02T)=Sof(H02U)=1-FVAR(2)
 Sof(H03Z)=Sof(C8B)=Sof(H4AA)=Sof(H4AB)=Sof(C9B)=Sof(H1AA)=Sof(H1AB)=Sof(C10B)=
 Sof(H3AA)=Sof(H3AB)=Sof(C11B)=Sof(H2AA)=Sof(H2AB)=Sof(H02R)=Sof(H02S)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C1F(H010), C7F(H00W), C20F(H00T), C26F(H016), C1A(H017), C1B(H00S), C1D(H00L),
  C7A(H00X), C7B(H0GA), C7B(H03Z), C7D(H8), C7E(H0), C20A(H014), C20B(H01Z),
 C20D(H00U), C26A(H013), C26B(H012), C26D(H02C)
3.b Secondary CH2 refined with riding coordinates:
 C2F(H6CA,HA), C3F(H4EA,HY), C4F(H1EA,HW), C5F(H9DA,HS), C6F(H3DA,HL),
 C8F(H1DA,HJ), C9F(H5DA,HN), C10F(H0FA,H6EA), C11F(H5EA,H9EA), C12F(H2DA,HK),
 C21F(H0DA,HI), C22F(H3EA,HX), C23F(H7DA,HR), C24F(H4DA,HM), C25F(H,H5CA),
 C27F(H9CA,HH), C28F(H0EA,HV), C29F(H5FA,H7EA), C30F(H6FA,H8EA), C31F(H7CA,HF),
 C2A(H5BA,HQ), C2B(H03U,H03V), C2D(H01C,H01D), C3A(H02X,H02Y), C3B(H03W,H03X),
 C3D(H02F,H02H), C4A(H8BA,HU), C4B(H03Y,H7FA), C4D(H03I,H03J), C5A(H02,HP),
 C5B(H03M,H03N), C5D(H03K,H03L), C6A(H01X,H01Y), C6B(H00C,H00D), C6D(H03G,H03H),
  C8A(H0BA,HD), C8B(H4AA,H4AB), C8C(H5AA,H5AB), C8D(H01Q,H01R), C8D(H01N,H01P),
 C9A(H6BA,HT), C9B(H1AA,H1AB), C9C(H0AA,H0AB), C9D(H7A,H7B), C9E(H2A,H2B),
 C10A(H03,HZ), C10B(H3AA,H3AB), C10C(H7AA,H7AB), C10D(H6A,H6B), C10E(H3A,H3B),
 C11A(H1BA,HE), C11B(H2AA,H2AB), C11C(H6AA,H6AB), C11D(H1A,H1B), C11E(H8AA,
 H8AB), C12A(H2BA,HG), C12B(H02T,H02U), C12B(H02R,H02S), C12D(H5A,H5B),
 C12E(H4A,H4B), C21A(H02Z,HO), C21B(H01V,H01W), C21D(H01A,H01B), C22A(H2CA,
 H4FA), C22B(H03S,H03T), C22D(H02A,H02B), C23A(H4CA,H9FA), C23B(H03Q,H03R),
 C23D(H01K,H01M), C24A(H1CA,H3FA), C24B(H03O,H03P), C24D(H01G,H01H), C25A(H9AA,
 HC), C25B(H02M,H02N), C25D(H01E,H01F), C27A(H01,HB), C27B(H00A,H00B),
 C27D(H01I,H01J), C28A(H0CA,H2FA), C28B(H02K,H02L), C28D(H03A,H03B), C29A(H1FA,
 H9BA), C29B(H02I,H02J), C29D(H03E,H03F), C30A(H3CA,H8FA), C30B(H02O,H02P),
 C30D(H03C,H03D), C31A(H02V,H02W), C31B(H01T,H01U), C31D(H02D,H02E)
3.c Aromatic/amide H refined with riding coordinates:
 C15F(H8CA), C16F(H6DA), C17F(H8DA), C18F(H2EA), C15A(H4BA), C15B(H01S),
 C15D(H02G), C16A(H3BA), C16B(H026), C16D(H01L), C17A(H033), C17B(H02Q),
 C17D(H01O), C18A(H7BA), C18B(H024), C18D(H027)
;
_shelx_res_checksum              47321
_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 1.498
_oxdiff_exptl_absorpt_empirical_full_min 0.877