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_1552473
_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         'C36 H58 N2 P4, 2(C F3 O3 S)'
_chemical_formula_sum            'C38 H58 F6 N2 O6 P4 S2'
_chemical_formula_weight         940.86
_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             2018-11-05
_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                87.895(6)
_cell_angle_beta                 80.107(6)
_cell_angle_gamma                86.923(6)
_cell_formula_units_Z            1
_cell_length_a                   9.5582(7)
_cell_length_b                   9.6936(8)
_cell_length_c                   11.8527(8)
_cell_measurement_reflns_used    2856
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.4640
_cell_measurement_theta_min      4.6670
_cell_volume                     1079.88(14)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_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   -111.00 -74.00   0.50    4.00    --  -38.50 -38.00-180.00   74
  2  \w    -61.00  31.00   0.50    4.00    --  -38.50  57.00-120.00  184
  3  \w   -109.00 -16.00   0.50    4.00    --  -38.50 -57.00  90.00  186
  4  \w    -55.00  29.00   0.50    4.00    --  -38.50  38.00   0.00  168
  5  \w     46.00  73.00   0.50    4.00    --   42.25 -99.00-120.00   54
  6  \w      1.00  70.00   0.50    4.00    --   42.25 -99.00  60.00  138
  7  \w     39.00  84.00   0.50   16.00    --  111.00 -94.00   0.00   90
  8  \w     39.00 126.00   0.50   16.00    --  111.00 -30.00  30.00  174
  9  \w     84.00 117.00   0.50   16.00    --  111.00 -77.00  90.00   66
 10  \w     39.00 113.00   0.50   16.00    --  111.00-125.00 -60.00  148
 11  \w     30.00  85.00   0.50   16.00    --  111.00 -94.00  60.00  110
 12  \w     39.00 176.00   0.50   16.00    --  111.00   0.00 -90.00  274
 13  \w     59.00 135.00   0.50   16.00    --  111.00 -45.00-150.00  152
 14  \w    104.00 131.00   0.50   16.00    --  111.00 -30.00 -60.00   54
 15  \w     96.00 123.00   0.50   16.00    --  111.00 125.00 -90.00   54
 16  \w     68.00 116.00   0.50   16.00    --  111.00 -30.00 120.00   96
 17  \w     71.00 121.00   0.50   16.00    --  111.00-125.00  60.00  100
 18  \w     53.00 103.00   0.50   16.00    --  111.00-125.00 -90.00  100
 19  \w     75.00 110.00   0.50   16.00    --  111.00-125.00   0.00   70
 20  \w     52.00 107.00   0.50   16.00    --  111.00 -94.00  90.00  110
 21  \w    102.00 149.00   0.50   16.00    --  111.00  45.00 -60.00   94
 22  \w     72.00 134.00   0.50   16.00    --  111.00 -45.00  60.00  124
 23  \w     67.00  81.50   0.50   16.00    --  111.00-125.00-120.00   29
;
_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      -0.1488090000
_diffrn_orient_matrix_UB_12      -0.0211829000
_diffrn_orient_matrix_UB_13      0.0704627000
_diffrn_orient_matrix_UB_21      -0.0616560000
_diffrn_orient_matrix_UB_22      -0.0046122000
_diffrn_orient_matrix_UB_23      -0.1115799000
_diffrn_orient_matrix_UB_31      0.0297425000
_diffrn_orient_matrix_UB_32      -0.1577338000
_diffrn_orient_matrix_UB_33      -0.0024746000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7302
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.310
_diffrn_reflns_theta_min         3.787
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.155
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.568
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       needle
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         7302
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0700
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1529P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1808
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5821
_reflns_number_total             7302
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.7958\% 
 around [0.98 0.05 0.21] (reciprocal) or [1.00 -0.00 0.00] (direct)
;
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           19OTf2
_cod_database_code               1552473
_chemical_oxdiff_formula         C38H58F6N2O6P4S2
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5907(16) 0.4093(16)
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. Uiso/Uaniso restraints and constraints
S1A \\sim F1A \\sim F2A \\sim F3A \\sim O2A \\sim O1 \\sim O3A \\sim C19A \\sim
S1B \\sim F1B \\sim F2B \\sim F3B \\sim O3B \\sim O2B \\sim C19B: within 2A
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(S1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O3B)=Sof(O2B)=Sof(C19B)=1-FVAR(1)
 Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O2A)=Sof(O3A)=Sof(C19A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              69739
_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 3.191
_oxdiff_exptl_absorpt_empirical_full_min 0.630
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2