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_1552461
_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         'C F3 O3 S, C30 H51 N P3'
_chemical_formula_sum            'C31 H51 F3 N O3 P3 S'
_chemical_formula_weight         667.69
_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             2018-01-16
_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                74.779(3)
_cell_angle_beta                 67.319(3)
_cell_angle_gamma                84.620(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9026(4)
_cell_length_b                   12.5147(3)
_cell_length_c                   14.0376(4)
_cell_measurement_reflns_used    10873
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3190
_cell_measurement_theta_min      3.5100
_cell_volume                     1705.16(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.985
_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    -58.00  33.00   0.50    4.00    --  -38.50  38.00 -60.00  182
  2  \w    -67.00 -17.00   0.50    4.00    --  -38.50 125.00-180.00  100
  3  \w   -106.00 -17.00   0.50    4.00    --  -38.50 -57.00   0.00  178
  4  \w    -64.00  32.00   0.50    4.00    --  -38.50  57.00 150.00  192
  5  \w     46.00  98.00   0.50    4.00    --   42.75-125.00 -30.00  104
  6  \w     44.00  71.00   0.50   16.00    --  111.00 -94.00  30.00   54
  7  \w     63.00 118.00   0.50   16.00    --  111.00-125.00   0.00  110
  8  \w     77.00 104.00   0.50   16.00    --  111.00-125.00 -30.00   54
  9  \w     77.00 121.00   0.50   16.00    --  111.00-125.00 -60.00   88
 10  \w     91.00 118.00   0.50   16.00    --  111.00-125.00-120.00   54
 11  \w     84.00 109.00   0.50   16.00    --  111.00 -94.00-150.00   50
 12  \w     78.00 107.00   0.50   16.00    --  111.00 -30.00 -90.00   58
 13  \w    101.00 128.00   0.50   16.00    --  111.00  30.00-180.00   54
 14  \w    109.00 175.00   0.50   16.00    --  111.00  45.00-180.00  132
 15  \w    136.00 163.00   0.50   16.00    --  111.00  45.00 -90.00   54
 16  \w     88.00 178.00   0.50   16.00    --  111.00  30.00-120.00  180
 17  \w     81.00 120.00   0.50   16.00    --  111.00 -30.00   0.00   78
 18  \w     68.00 120.00   0.50   16.00    --  111.00-125.00 120.00  104
 19  \w     42.00  80.00   0.50   16.00    --  111.00 -30.00   0.00   76
 20  \w     38.00  65.00   0.50   16.00    --  111.00 -30.00 -90.00   54
 21  \w     68.00 134.00   0.50   16.00    --  111.00 -30.00-180.00  132
 22  \w     48.00 126.00   0.50   16.00    --  111.00 -45.00-180.00  156
 23  \w     40.00 121.00   0.50   16.00    --  111.00-125.00-180.00  162
 24  \w     31.00 104.00   0.50   16.00    --  111.00 -94.00   0.00  146
 25  \w     43.00 121.00   0.50   16.00    --  111.00 -61.00 120.00  156
 26  \w     96.00 178.00   0.50   16.00    --  111.00  15.00 150.00  164
 27  \w     44.00  97.00   0.50   16.00    --  111.00-125.00 150.00  106
 28  \w     34.00  90.00   0.50   16.00    --  111.00 -94.00  60.00  112
 29  \w     31.00  56.00   0.50   16.00    --  111.00 -94.00-150.00   50
;
_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      -0.1399280000
_diffrn_orient_matrix_UB_12      0.0014365000
_diffrn_orient_matrix_UB_13      -0.0029898000
_diffrn_orient_matrix_UB_21      0.0105663000
_diffrn_orient_matrix_UB_22      -0.1245917000
_diffrn_orient_matrix_UB_23      0.0039582000
_diffrn_orient_matrix_UB_31      -0.0613478000
_diffrn_orient_matrix_UB_32      -0.0274106000
_diffrn_orient_matrix_UB_33      0.1226288000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.650
_diffrn_reflns_theta_min         3.521
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.581
_exptl_absorpt_correction_T_max  0.904
_exptl_absorpt_correction_T_min  0.721
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0620P)^2^+0.6572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6566
_reflns_number_total             7087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           10OTf
_cod_original_cell_volume        1705.17(10)
_cod_database_code               1552461
_chemical_oxdiff_formula         'C62 H104 F6 N2 O6 P2 S6 '
_reflns_odcompleteness_completeness 99.90
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C8(H8), C19(H19), C25(H25)
2.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), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
2.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              16547
_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 1.466
_oxdiff_exptl_absorpt_empirical_full_min 0.760