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_1552476
_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 Au2 N2 P6, 2(C F3 O3 S)'
_chemical_formula_sum            'C60 H96 Au2 F6 N2 O6 P6 S2'
_chemical_formula_weight         1699.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-12
_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                 115.147(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.8614(6)
_cell_length_b                   16.4069(4)
_cell_length_c                   26.8718(6)
_cell_measurement_reflns_used    14691
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      75.6370
_cell_measurement_theta_min      3.5290
_cell_volume                     8724.8(4)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_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 0.983
_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  32.00   0.50    1.00    --  -38.50  38.00  30.00   96
  2  \w     17.00 105.00   0.50    1.00    --   42.50  57.00  90.00  176
  3  \w     96.00 131.00   0.50    4.00    --  111.00 125.00  60.00   70
  4  \w    118.00 169.00   0.50    4.00    --  111.00 125.00  90.00  102
  5  \w     95.00 173.00   0.50    4.00    --  111.00 125.00 120.00  156
  6  \w    142.00 178.00   0.50    4.00    --  111.00  30.00-120.00   72
  7  \w     94.00 144.00   0.50    4.00    --  111.00 125.00-180.00  100
  8  \w     59.00 129.00   0.50    4.00    --  111.00 -45.00 120.00  140
  9  \w     59.00 100.00   0.50    4.00    --  111.00-100.00 131.00   82
 10  \w     40.00  73.00   0.50    4.00    --  111.00-125.00 150.00   66
 11  \w     41.00  90.00   0.50    4.00    --  111.00 -94.00  90.00   98
 12  \w     38.00 109.00   0.50    4.00    --  111.00 -94.00  60.00  142
 13  \w     42.00 115.00   0.50    4.00    --  111.00-125.00 -60.00  146
 14  \w     62.00 106.00   0.50    4.00    --  111.00 -94.00-180.00   88
 15  \w    -30.00  63.00   0.50    1.00    --   42.50 -38.00-180.00  186
 16  \w    -91.00 -47.00   0.50    1.00    --  -38.50 125.00  90.00   88
;
_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      -0.0112294000
_diffrn_orient_matrix_UB_12      0.0892242000
_diffrn_orient_matrix_UB_13      -0.0198538000
_diffrn_orient_matrix_UB_21      -0.0618392000
_diffrn_orient_matrix_UB_22      0.0052773000
_diffrn_orient_matrix_UB_23      0.0133001000
_diffrn_orient_matrix_UB_31      0.0458901000
_diffrn_orient_matrix_UB_32      0.0286788000
_diffrn_orient_matrix_UB_33      0.0586794000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23941
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.773
_diffrn_reflns_theta_min         3.478
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.144
_exptl_absorpt_correction_T_max  0.405
_exptl_absorpt_correction_T_min  0.222
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3408
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.407
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         9046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+37.3310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8619
_reflns_number_total             9046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           9aAuOTf
_cod_database_code               1552476
_reflns_odcompleteness_completeness 99.95
_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
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:
 C13(H13), C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              80112
_shelx_fab_checksum              41236
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'