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_1552466
_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         'C25 H20 N5 P5'
_chemical_formula_sum            'C25 H20 N5 P5'
_chemical_formula_weight         545.31
_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   difmap
_audit_creation_date             2017-04-11
_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                90
_cell_angle_beta                 92.3033(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.88106(6)
_cell_length_b                   19.32439(15)
_cell_length_c                   14.68865(11)
_cell_measurement_reflns_used    10202
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.3250
_cell_measurement_theta_min      4.5770
_cell_volume                     2518.85(3)
_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 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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   1.00   0.50    0.75    --  -38.50  57.00 150.00  132
  2  \w   -107.00 -43.00   0.50    0.75    --  -38.50 -57.00 -30.00  128
  3  \w     24.00  93.00   0.50    0.75    --   42.75-125.00 -60.00  138
  4  \w     41.00 128.00   0.50    3.00    --  111.00 -45.00-180.00  174
  5  \w     88.00 134.00   0.50    3.00    --  111.00  30.00 -60.00   92
  6  \w     86.00 168.00   0.50    3.00    --  111.00  61.00 -30.00  164
  7  \w    142.00 167.00   0.50    3.00    --  111.00  15.00  90.00   50
  8  \w     93.00 147.00   0.50    3.00    --  111.00  45.00  60.00  108
  9  \w     81.00 108.00   0.50    3.00    --  111.00  15.00  90.00   54
 10  \w     75.00 139.00   0.50    3.00    --  111.00  15.00 150.00  128
 11  \w     31.00 106.00   0.50    3.00    --  111.00 -94.00  30.00  150
 12  \w     91.00 120.00   0.50    3.00    --  111.00-125.00 -90.00   58
 13  \w     39.00  76.00   0.50    3.00    --  111.00-125.00 -90.00   74
 14  \w     31.00  58.00   0.50    3.00    --  111.00 -94.00-180.00   54
 15  \w     60.00 106.00   0.50    0.75    --   42.75  38.00-150.00   92
 16  \w     97.00 150.00   0.50    3.00    --  111.00  77.00-180.00  106
 17  \w    137.00 170.00   0.50    3.00    --  111.00 125.00-180.00   66
 18  \w     95.00 122.00   0.50    3.00    --  111.00 125.00-180.00   54
;
_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      -0.0431062000
_diffrn_orient_matrix_UB_12      0.0184377000
_diffrn_orient_matrix_UB_13      0.0976391000
_diffrn_orient_matrix_UB_21      0.1341725000
_diffrn_orient_matrix_UB_22      0.0504359000
_diffrn_orient_matrix_UB_23      0.0082612000
_diffrn_orient_matrix_UB_31      -0.1014937000
_diffrn_orient_matrix_UB_32      0.0588585000
_diffrn_orient_matrix_UB_33      -0.0376902000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14356
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.533
_diffrn_reflns_theta_min         3.782
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.577
_exptl_absorpt_correction_T_max  0.781
_exptl_absorpt_correction_T_min  0.621
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.101
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0348P)^2^+1.0206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5073
_reflns_number_total             5232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           13
_cod_original_cell_volume        2518.84(3)
_cod_database_code               1552466
_chemical_oxdiff_formula         'C100 H80 N20 P20 '
_chemical_oxdiff_usercomment     (PyrP)5
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_shelx_res_checksum              16421
_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 1.247
_oxdiff_exptl_absorpt_empirical_full_min 0.750