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_1552465
_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 Cu2 N2 P6, 2(C F3 O3 S), 4(C H2 Cl2)'
_chemical_formula_sum            'C64 H104 Cl8 Cu2 F6 N2 O6 P6 S2'
_chemical_formula_weight         1772.11
_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             2018-12-11
_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                113.879(2)
_cell_angle_beta                 109.229(2)
_cell_angle_gamma                93.1122(18)
_cell_formula_units_Z            1
_cell_length_a                   12.3686(3)
_cell_length_b                   13.7415(3)
_cell_length_c                   13.9572(3)
_cell_measurement_reflns_used    12945
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1470
_cell_measurement_theta_min      3.6130
_cell_volume                     1999.20(9)
_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 0.988
_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    -23.00   4.00   0.50    0.75    --   42.75 -38.00 -30.00   54
  2  \w     40.00  65.00   0.50    0.75    --   42.75 -38.00 -30.00   50
  3  \w      1.00  35.00   0.50    0.75    --   42.75 -99.00-150.00   68
  4  \w     38.00  98.00   0.50    0.75    --   42.75-125.00-180.00  120
  5  \w     44.00  73.00   0.50    3.00    --  111.00 -94.00 -90.00   58
  6  \w     84.00 109.00   0.50    3.00    --  111.00 -94.00 -90.00   50
  7  \w     80.00 118.00   0.50    3.00    --  111.00-125.00-120.00   76
  8  \w    104.00 132.00   0.50    3.00    --  111.00 -77.00-180.00   56
  9  \w     78.00 155.00   0.50    3.00    --  111.00 -15.00-150.00  154
 10  \w    127.00 156.00   0.50    3.00    --  111.00 -15.00 -30.00   58
 11  \w    116.00 141.00   0.50    3.00    --  111.00 -77.00  60.00   50
 12  \w     96.00 121.00   0.50    3.00    --  111.00-125.00 120.00   50
 13  \w     75.00 121.00   0.50    3.00    --  111.00-125.00  30.00   92
 14  \w     65.00  96.00   0.50    3.00    --  111.00 -77.00  60.00   62
 15  \w     62.00  88.00   0.50    3.00    --  111.00 -94.00  60.00   52
 16  \w     52.00  79.00   0.50    3.00    --  111.00 -94.00 -30.00   54
 17  \w     40.00 131.00   0.50    3.00    --  111.00 -45.00   0.00  182
 18  \w     73.00 114.00   0.50    3.00    --  111.00-125.00-150.00   82
 19  \w     50.00 104.00   0.50    3.00    --  111.00-125.00-180.00  108
 20  \w     52.00 104.00   0.50    3.00    --  111.00 -94.00-120.00  104
 21  \w     41.00 130.00   0.50    3.00    --  111.00 -45.00-120.00  178
 22  \w     41.00 105.00   0.50    3.00    --  111.00 -94.00  30.00  128
 23  \w     47.00  74.00   0.50    3.00    --  111.00-125.00 120.00   54
 24  \w     41.00 133.00   0.50    3.00    --  111.00 -45.00 120.00  184
 25  \w     31.00  75.00   0.50    3.00    --  111.00 -15.00 -30.00   88
 26  \w     31.00  70.00   0.50    3.00    --  111.00 -15.00-150.00   78
 27  \w    133.00 165.00   0.50    3.00    --  111.00  77.00-120.00   64
 28  \w     33.00 155.00   0.50    3.00    --  111.00 -15.00  90.00  244
 29  \w     21.00 113.00   0.50    0.75    --   42.75  38.00 150.00  184
 30  \w    -62.00  32.00   0.50    0.75    --  -38.50  57.00  30.00  188
 31  \w   -108.00 -14.00   0.50    0.75    --  -38.50 -57.00-120.00  188
;
_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      -0.0792652000
_diffrn_orient_matrix_UB_12      -0.0185931000
_diffrn_orient_matrix_UB_13      0.0588230000
_diffrn_orient_matrix_UB_21      -0.0131187000
_diffrn_orient_matrix_UB_22      -0.1241046000
_diffrn_orient_matrix_UB_23      -0.0638986000
_diffrn_orient_matrix_UB_31      0.1086671000
_diffrn_orient_matrix_UB_32      0.0053986000
_diffrn_orient_matrix_UB_33      0.0977740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19879
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.510
_diffrn_reflns_theta_min         3.604
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.255
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.383
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.307
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0385P)^2^+1.1409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7795
_reflns_number_total             8310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           9aCuOTf
_cod_database_code               1552465
_chemical_oxdiff_formula         'C64 H96 Cl8 Cu2 F6 N2 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, All C(H,H,H,H) groups
2. Others
 Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19C)=Sof(H19D)=Sof(H20C)=Sof(H20D)=
 Sof(C21B)=Sof(H21C)=Sof(H21D)=Sof(C22B)=Sof(H22C)=Sof(H22D)=Sof(H23C)=
 Sof(H23D)=1-FVAR(1)
 Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(H19B)=Sof(H20A)=Sof(H20B)=
 Sof(C21A)=Sof(H21A)=Sof(H21B)=Sof(C22A)=Sof(H22A)=Sof(H22B)=Sof(H23A)=
 Sof(H23B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C18A(H18A), C18B(H18B), C24(H24)
3.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), C19A(H19A,H19B),
 C19B(H19C,H19D), C20(H20C,H20D), C20(H20A,H20B), C21A(H21A,H21B), C21B(H21C,
 H21D), C22A(H22A,H22B), C22B(H22C,H22D), C23(H23A,H23B), C23(H23C,H23D),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B),
  C31(H31A,H31B), C32(H32A,H32B)
3.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              81966
_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 1.231
_oxdiff_exptl_absorpt_empirical_full_min 0.799