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_1552464
_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         'C58 H96 Ag2 N2 P6, 2(C F3 O3 S), 2(C2 H3 N)'
_chemical_formula_sum            'C64 H102 Ag2 F6 N4 O6 P6 S2'
_chemical_formula_weight         1603.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-09-29
_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                 102.677(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1473(3)
_cell_length_b                   15.0565(4)
_cell_length_c                   20.4248(7)
_cell_measurement_reflns_used    10176
_cell_measurement_temperature    99.97(13)
_cell_measurement_theta_max      74.2530
_cell_measurement_theta_min      3.6770
_cell_volume                     3644.55(19)
_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(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.980
_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    -65.00  32.00   0.50    5.00    --  -38.50  57.00 -30.00  194
  2  \w    -56.00  34.00   0.50    5.00    --  -38.50  38.00 120.00  180
  3  \w   -109.00 -15.00   0.50    5.00    --  -38.50 -57.00-180.00  188
  4  \w      4.00  59.00   0.50    5.00    --   42.50 -99.00  30.00  110
  5  \w     26.00  93.00   0.50    5.00    --   42.50-125.00 150.00  134
  6  \w     45.00  84.00   0.50   20.00    --  111.00 -94.00 -30.00   78
  7  \w     90.00 121.00   0.50   20.00    --  111.00-125.00 -30.00   62
  8  \w     47.00  97.00   0.50   20.00    --  111.00 -45.00 -60.00  100
  9  \w     44.00 135.00   0.50   20.00    --  111.00 -30.00  60.00  182
 10  \w     41.00 133.00   0.50   20.00    --  111.00 -61.00-150.00  184
 11  \w    114.00 177.00   0.50   20.00    --  111.00  30.00 -90.00  126
 12  \w     45.00  79.00   0.50   20.00    --  111.00 -77.00-180.00   68
 13  \w     90.00 117.00   0.50   20.00    --  111.00 -77.00-180.00   54
 14  \w     60.00 121.00   0.50   20.00    --  111.00-125.00-120.00  122
 15  \w     39.00  73.00   0.50   20.00    --  111.00-125.00 -30.00   68
 16  \w    100.00 174.00   0.50   20.00    --  111.00  30.00 -30.00  148
 17  \w     87.00 120.00   0.50   20.00    --  111.00-125.00  90.00   66
 18  \w     59.00  84.00   0.50   20.00    --  111.00-125.00 120.00   50
 19  \w     47.00  74.00   0.50   20.00    --  111.00-125.00  90.00   54
 20  \w     45.00  78.00   0.50   20.00    --  111.00 -30.00 150.00   66
 21  \w     87.00 123.00   0.50   20.00    --  111.00 -30.00 150.00   72
 22  \w     62.00  94.00   0.50   20.00    --  111.00 -94.00   0.00   64
 23  \w     43.00  43.50   0.50   20.00    --  111.00 -15.00   0.00    1
;
_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      -0.1181585000
_diffrn_orient_matrix_UB_12      0.0033961000
_diffrn_orient_matrix_UB_13      -0.0467044000
_diffrn_orient_matrix_UB_21      0.0501436000
_diffrn_orient_matrix_UB_22      -0.0315608000
_diffrn_orient_matrix_UB_23      -0.0590416000
_diffrn_orient_matrix_UB_31      -0.0204090000
_diffrn_orient_matrix_UB_32      -0.0972958000
_diffrn_orient_matrix_UB_33      0.0175383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23315
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.127
_diffrn_reflns_theta_min         3.679
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.637
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.632
_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    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.022
_refine_diff_density_max         1.330
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0631P)^2^+1.5538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6108
_reflns_number_total             7033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           9aAgOTf
_cod_original_cell_volume        3644.55(18)
_cod_database_code               1552464
_chemical_oxdiff_formula         'C92 H204 Ag4 F12 N44 O12 S16 P1 '
_reflns_odcompleteness_completeness 98.19
_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), C18(H18), C24(H24)
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), C19(H19A,H19B),
 C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B),
  C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17)
2.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_res_checksum              6649
_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 3.513
_oxdiff_exptl_absorpt_empirical_full_min 0.630