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_1552470
_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 H54 N P3, 2(C F3 O3 S)'
_chemical_formula_sum            'C33 H54 F6 N O6 P3 S2'
_chemical_formula_weight         831.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-24
_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                90
_cell_angle_beta                 109.4646(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.83650(10)
_cell_length_b                   21.99929(12)
_cell_length_c                   13.99782(10)
_cell_measurement_reflns_used    30237
_cell_measurement_temperature    99.97(12)
_cell_measurement_theta_max      76.4420
_cell_measurement_theta_min      3.8920
_cell_volume                     4017.32(5)
_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      99.97(12)
_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 0.994
_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     18.00  56.00   0.50    1.50    --   42.62 -37.00  50.00   76
  2  \w     44.00  71.00   0.50    1.50    --   42.62  57.00 -90.00   54
  3  \w     96.00 123.00   0.50    6.00    --  111.00 -30.00 -60.00   54
  4  \w     94.00 138.00   0.50    6.00    --  111.00 -77.00 -90.00   88
  5  \w    111.00 136.00   0.50    6.00    --  111.00 -77.00-150.00   50
  6  \w     95.00 121.00   0.50    6.00    --  111.00-125.00-180.00   52
  7  \w     89.00 121.00   0.50    6.00    --  111.00-125.00 -90.00   64
  8  \w     56.00 107.00   0.50    6.00    --  111.00 -94.00 -90.00  102
  9  \w     56.00  83.00   0.50    6.00    --  111.00 -77.00 -90.00   54
 10  \w     44.00  73.00   0.50    6.00    --  111.00 -94.00-120.00   58
 11  \w     39.00 113.00   0.50    6.00    --  111.00-125.00-120.00  148
 12  \w     41.00  74.00   0.50    6.00    --  111.00 -45.00-150.00   66
 13  \w     41.00 131.00   0.50    6.00    --  111.00 -45.00 -90.00  180
 14  \w     96.00 123.00   0.50    6.00    --  111.00  30.00   0.00   54
 15  \w    130.00 178.00   0.50    6.00    --  111.00  30.00   0.00   96
 16  \w    105.00 152.00   0.50    6.00    --  111.00 125.00-120.00   94
 17  \w    132.00 175.00   0.50    6.00    --  111.00 125.00 -90.00   86
 18  \w     91.00 176.00   0.50    6.00    --  111.00  45.00 -60.00  170
 19  \w     81.00 150.00   0.50    6.00    --  111.00 -15.00 120.00  138
 20  \w     52.00 156.00   0.50    6.00    --  111.00 -15.00 -60.00  208
 21  \w     56.00 118.00   0.50    6.00    --  111.00-125.00  90.00  124
 22  \w     48.00  99.00   0.50    6.00    --  111.00-125.00 120.00  102
 23  \w     50.00 121.00   0.50    6.00    --  111.00-125.00 150.00  142
 24  \w     42.00  70.00   0.50    6.00    --  111.00 -30.00 120.00   56
 25  \w     31.00  58.00   0.50    6.00    --  111.00 -15.00 120.00   54
 26  \w    -13.00  18.00   0.50    1.50    --   42.62 -57.00 -30.00   62
 27  \w     39.00 121.00   0.50    6.00    --  111.00-125.00  30.00  164
 28  \w     37.00  78.00   0.50    6.00    --  111.00 -77.00-150.00   82
 29  \w     52.00  88.00   0.50    6.00    --  111.00 -94.00-180.00   72
 30  \w     41.00  85.00   0.50    6.00    --  111.00-125.00-180.00   88
 31  \w    -70.00  35.00   0.50    1.50    --  -38.50  77.00 -90.00  210
 32  \w    -67.00  35.00   0.50    1.50    --  -38.50  77.00  30.00  204
 33  \w    -70.00  35.00   0.50    1.50    --  -38.50  77.00 150.00  210
;
_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      -0.1009078000
_diffrn_orient_matrix_UB_12      -0.0206793000
_diffrn_orient_matrix_UB_13      -0.0801763000
_diffrn_orient_matrix_UB_21      0.0363984000
_diffrn_orient_matrix_UB_22      0.0261823000
_diffrn_orient_matrix_UB_23      -0.0844074000
_diffrn_orient_matrix_UB_31      0.0491546000
_diffrn_orient_matrix_UB_32      -0.0615446000
_diffrn_orient_matrix_UB_33      -0.0091764000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44324
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.687
_diffrn_reflns_theta_min         3.891
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.944
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.594
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.472
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         8432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0447P)^2^+2.3518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8188
_reflns_number_total             8432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           11OTf2
_cod_database_code               1552470
_chemical_oxdiff_formula         'C84 H220 F40 N52 O8 S20 P1 '
_reflns_odcompleteness_completeness 99.99
_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 Aromatic/amide H refined with riding coordinates:
 C00R(H00R), C00U(H00U), C00Z(H00Z), C010(H010)
2.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              77884
_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 1.366
_oxdiff_exptl_absorpt_empirical_full_min 0.679