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_1552463
_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         'C21 H40 N P3'
_chemical_formula_sum            'C21 H40 N P3'
_chemical_formula_weight         399.45
_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             2018-08-08
_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                73.202(3)
_cell_angle_beta                 86.167(3)
_cell_angle_gamma                72.923(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9088(3)
_cell_length_b                   11.2925(4)
_cell_length_c                   14.4882(6)
_cell_measurement_reflns_used    10447
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4860
_cell_measurement_theta_min      3.1640
_cell_volume                     1183.89(8)
_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 10.5700
_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   -109.00 -12.00   0.50    1.00    --  -38.50 -57.00-180.00  194
  2  \w    -65.00  32.00   0.50    1.00    --  -38.50  57.00 -30.00  194
  3  \w     20.00 115.00   0.50    1.00    --   42.75  38.00-150.00  190
  4  \w      1.00  83.00   0.50    1.00    --   42.75 -99.00 120.00  164
  5  \w     23.00  98.00   0.50    1.00    --   42.75-125.00 120.00  150
  6  \w    -30.00  65.00   0.50    1.00    --   42.75 -38.00  30.00  190
  7  \w     31.00 156.00   0.50    4.00    --  111.00 -15.00-120.00  250
  8  \w     30.00 109.00   0.50    4.00    --  111.00 -94.00  60.00  158
  9  \w     94.00 178.00   0.50    4.00    --  111.00 125.00 120.00  168
 10  \w     87.00 178.00   0.50    4.00    --  111.00  45.00-120.00  182
 11  \w     87.00 178.00   0.50    4.00    --  111.00  45.00-150.00  182
 12  \w     37.00 142.00   0.50    4.00    --  111.00 -77.00  90.00  210
 13  \w     40.00 135.00   0.50    4.00    --  111.00 -45.00 -90.00  190
 14  \w     87.00 178.00   0.50    4.00    --  111.00  30.00 150.00  182
 15  \w     30.00 109.00   0.50    4.00    --  111.00 -94.00 -60.00  158
 16  \w     39.00 121.00   0.50    4.00    --  111.00-125.00 120.00  164
 17  \w     39.00 121.00   0.50    4.00    --  111.00-125.00 -60.00  164
 18  \w     39.00 121.00   0.50    4.00    --  111.00-125.00  30.00  164
 19  \w     39.00 121.00   0.50    4.00    --  111.00-125.00 -90.00  164
 20  \w     83.00 175.00   0.50    4.00    --  111.00  61.00  60.00  184
 21  \w     75.00 121.00   0.50    4.00    --  111.00-125.00-180.00   92
 22  \w     41.00 135.00   0.50    4.00    --  111.00 -45.00  60.00  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      -0.1565605000
_diffrn_orient_matrix_UB_12      0.1087817000
_diffrn_orient_matrix_UB_13      0.0189253000
_diffrn_orient_matrix_UB_21      -0.0299919000
_diffrn_orient_matrix_UB_22      0.0621726000
_diffrn_orient_matrix_UB_23      -0.1094646000
_diffrn_orient_matrix_UB_31      -0.1270010000
_diffrn_orient_matrix_UB_32      -0.0802132000
_diffrn_orient_matrix_UB_33      -0.0009884000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14550
_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         76.921
_diffrn_reflns_theta_min         3.187
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.319
_exptl_absorpt_correction_T_max  0.844
_exptl_absorpt_correction_T_min  0.574
_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    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.397
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         4930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0347P)^2^+0.4663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4861
_reflns_number_total             4930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           9c
_cod_original_cell_volume        1183.90(8)
_cod_database_code               1552463
_chemical_oxdiff_formula         'C42 H80 N2 P6 '
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C)
;
_shelx_res_checksum              5024
_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 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.613