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_1552474
_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         'C26 H50 P3, C F3 O3 S'
_chemical_formula_sum            'C27 H50 F3 O3 P3 S'
_chemical_formula_weight         604.64
_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             2019-04-01
_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                114.387(3)
_cell_angle_beta                 96.369(2)
_cell_angle_gamma                116.073(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4338(4)
_cell_length_b                   12.5077(3)
_cell_length_c                   13.0479(4)
_cell_measurement_reflns_used    9857
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3810
_cell_measurement_theta_min      3.9730
_cell_volume                     1550.40(12)
_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 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     16.00 105.00   0.50    0.50    --   42.50  57.00  60.00  178
  2  \w     91.00 156.00   0.50    2.00    --  111.00  30.00  90.00  130
  3  \w    118.00 145.00   0.50    2.00    --  111.00  30.00   0.00   54
  4  \w     98.00 177.00   0.50    2.00    --  111.00  30.00 -60.00  158
  5  \w     98.00 147.00   0.50    2.00    --  111.00 125.00 -30.00   98
  6  \w     94.00 172.00   0.50    2.00    --  111.00  61.00 -30.00  156
  7  \w     87.00 113.00   0.50    2.00    --  111.00  30.00   0.00   52
  8  \w     85.00 170.00   0.50    2.00    --  111.00  61.00  30.00  170
  9  \w     91.00 127.00   0.50    2.00    --  111.00  45.00 120.00   72
 10  \w     88.00 128.00   0.50    2.00    --  111.00 -61.00   0.00   80
 11  \w     83.00 118.00   0.50    2.00    --  111.00-125.00  60.00   70
 12  \w     91.00 121.00   0.50    2.00    --  111.00-125.00 120.00   60
 13  \w     70.00  97.00   0.50    0.50    --   42.50-125.00   0.00   54
 14  \w     25.00  56.00   0.50    0.50    --   42.50-125.00   0.00   62
 15  \w     41.00  68.00   0.50    2.00    --  111.00-125.00 120.00   54
 16  \w     46.00  81.00   0.50    2.00    --  111.00 -61.00   0.00   70
 17  \w     85.00 142.00   0.50    2.00    --  111.00 -77.00 -60.00  114
 18  \w     89.00 121.00   0.50    2.00    --  111.00-125.00 -60.00   64
 19  \w     84.00 109.00   0.50    2.00    --  111.00 -94.00 -90.00   50
 20  \w     84.00 139.00   0.50    2.00    --  111.00 -61.00-120.00  110
 21  \w     61.00 109.00   0.50    0.50    --   42.50  38.00-180.00   96
 22  \w     52.00  81.00   0.50    2.00    --  111.00 -61.00-120.00   58
 23  \w     38.00  64.00   0.50    2.00    --  111.00 -94.00 -90.00   52
 24  \w     64.00 121.00   0.50    2.00    --  111.00-125.00-120.00  114
 25  \w     46.00 116.00   0.50    2.00    --  111.00-125.00-180.00  140
 26  \w     39.00 103.00   0.50    2.00    --  111.00-125.00 -90.00  128
 27  \w     40.00  91.00   0.50    2.00    --  111.00-125.00-150.00  102
 28  \w     37.00  65.00   0.50    2.00    --  111.00 -77.00 -60.00   56
 29  \w    -81.00  -7.00   0.50    0.50    --  -38.50 125.00-180.00  148
 30  \w    -32.00  -3.00   0.50    0.50    --  -38.50 125.00-120.00   58
 31  \w    -84.00 -59.00   0.50    0.50    --  -38.50 125.00-120.00   50
 32  \w   -101.00 -16.00   0.50    0.50    --  -38.50 -77.00 120.00  170
;
_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      -0.0587161000
_diffrn_orient_matrix_UB_12      -0.1507258000
_diffrn_orient_matrix_UB_13      -0.1029883000
_diffrn_orient_matrix_UB_21      -0.1203272000
_diffrn_orient_matrix_UB_22      -0.0038167000
_diffrn_orient_matrix_UB_23      -0.0509783000
_diffrn_orient_matrix_UB_31      0.0623468000
_diffrn_orient_matrix_UB_32      0.0541695000
_diffrn_orient_matrix_UB_33      -0.0778547000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15021
_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         76.714
_diffrn_reflns_theta_min         3.983
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.770
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6454
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0378P)^2^+0.3201P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5907
_reflns_number_total             6454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           20OTf
_cod_original_cell_volume        1550.40(9)
_cod_database_code               1552474
_chemical_oxdiff_formula         'C38 H100 F6 N16 O6 P6 S2 '
_reflns_odcompleteness_completeness 100.00
_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:
 C1(H1), C7(H7), C14(H14), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B)
2.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              40793
_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 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.831