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_1552459
_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         'C15 H18 N5 P'
_chemical_formula_sum            'C15 H18 N5 P'
_chemical_formula_weight         299.31
_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   difmap
_audit_creation_date             2016-07-26
_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                89.776(2)
_cell_angle_beta                 85.729(3)
_cell_angle_gamma                61.439(3)
_cell_formula_units_Z            4
_cell_length_a                   8.4080(3)
_cell_length_b                   8.7414(2)
_cell_length_c                   24.3551(7)
_cell_measurement_reflns_used    9388
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.2840
_cell_measurement_theta_min      3.6360
_cell_volume                     1566.82(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 10.5700
_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     38.00 115.00   0.50    0.50    --   42.75  38.00   0.00  154
  2  \w    137.00 164.00   0.50    1.00    --  111.00  30.00 -90.00   54
  3  \w    136.00 177.00   0.50    1.00    --  111.00  30.00-120.00   82
  4  \w    102.00 133.00   0.50    1.00    --  111.00  45.00   0.00   62
  5  \w    137.00 178.00   0.50    1.00    --  111.00  61.00  60.00   82
  6  \w     95.00 136.00   0.50    1.00    --  111.00  30.00  60.00   82
  7  \w     89.00 178.00   0.50    1.00    --  111.00  45.00 120.00  178
  8  \w     84.00 129.00   0.50    1.00    --  111.00  61.00  60.00   90
  9  \w     91.00 127.00   0.50    1.00    --  111.00  30.00 -90.00   72
 10  \w    100.00 132.00   0.50    1.00    --  111.00  30.00-120.00   64
 11  \w     87.00 161.00   0.50    1.00    --  111.00  45.00-180.00  148
 12  \w     67.00  94.00   0.50    1.00    --  111.00 -94.00  30.00   54
 13  \w     85.00 121.00   0.50    1.00    --  111.00-125.00  30.00   72
 14  \w     89.00 120.00   0.50    1.00    --  111.00-125.00   0.00   62
 15  \w     78.00 127.00   0.50    1.00    --  111.00 -45.00  90.00   98
 16  \w     64.00  91.00   0.50    1.00    --  111.00 -94.00 150.00   54
 17  \w     59.00 121.00   0.50    1.00    --  111.00-125.00 120.00  124
 18  \w     41.00  72.00   0.50    1.00    --  111.00 -45.00  90.00   62
 19  \w     31.00  62.00   0.50    1.00    --  111.00 -94.00  30.00   62
 20  \w     39.00  69.00   0.50    1.00    --  111.00-125.00   0.00   60
 21  \w     46.00  86.00   0.50    1.00    --  111.00 -94.00 -60.00   80
 22  \w     41.00 124.00   0.50    1.00    --  111.00 -61.00 -60.00  166
 23  \w     78.00 121.00   0.50    1.00    --  111.00-125.00-150.00   86
 24  \w     55.00 109.00   0.50    1.00    --  111.00 -94.00-150.00  108
 25  \w     31.00  92.00   0.50    0.50    --   42.75-125.00 -90.00  122
 26  \w     30.00  57.00   0.50    0.50    --   42.75-125.00-180.00   54
 27  \w     32.00  85.00   0.50    1.00    --  111.00 -94.00 -90.00  106
 28  \w     31.00  90.00   0.50    0.50    --   42.75-125.00 120.00  118
 29  \w     30.00  93.00   0.50    1.00    --  111.00 -94.00 120.00  126
 30  \w   -124.00  40.00   0.50    0.50    --  -38.50   0.00   0.00  328
;
_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      0.1365292000
_diffrn_orient_matrix_UB_12      -0.1799096000
_diffrn_orient_matrix_UB_13      -0.0262968000
_diffrn_orient_matrix_UB_21      -0.1547572000
_diffrn_orient_matrix_UB_22      -0.0084857000
_diffrn_orient_matrix_UB_23      -0.0275976000
_diffrn_orient_matrix_UB_31      0.0350539000
_diffrn_orient_matrix_UB_32      0.0887489000
_diffrn_orient_matrix_UB_33      -0.0507497000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0200
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14923
_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         76.606
_diffrn_reflns_theta_min         3.642
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.772
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.269
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.623
_exptl_crystal_size_mid          0.575
_exptl_crystal_size_min          0.278
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0472P)^2^+0.6148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6309
_reflns_number_total             6482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           7
_cod_original_cell_volume        1566.81(9)
_cod_database_code               1552459
_chemical_oxdiff_formula         'C60 H72 N20 P4 '
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_shelx_res_checksum              6998
_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 1.515
_oxdiff_exptl_absorpt_empirical_full_min 0.583