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_1552472
_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_absolute_configuration ad
_chemical_formula_moiety         'C19 H18 N P3'
_chemical_formula_sum            'C19 H18 N P3'
_chemical_formula_weight         353.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-28
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.5691(4)
_cell_length_b                   10.80809(17)
_cell_length_c                   5.99320(10)
_cell_measurement_reflns_used    12900
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1870
_cell_measurement_theta_min      3.3070
_cell_volume                     1721.01(5)
_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 0.994
_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    -75.00  40.00   0.50    1.00    --  -38.50  19.00  90.00  230
  2  \w    -28.00  69.00   0.50    1.00    --   42.50 -57.00-120.00  194
  3  \w    -30.00  65.00   0.50    1.00    --   42.50 -38.00 120.00  190
  4  \w     23.00  98.00   0.50    1.00    --   42.50-125.00-180.00  150
  5  \w     20.00 115.00   0.50    1.00    --   42.50  38.00 -60.00  190
  6  \w      1.00  82.00   0.50    1.00    --   42.50 -99.00  30.00  162
  7  \w     39.00 121.00   0.50    4.00    --  111.00-125.00  30.00  164
  8  \w     31.00 156.00   0.50    4.00    --  111.00 -15.00-150.00  250
  9  \w     30.00 109.00   0.50    4.00    --  111.00 -94.00 150.00  158
 10  \w     87.00 178.00   0.50    4.00    --  111.00  45.00-180.00  182
 11  \w     37.00 142.00   0.50    4.00    --  111.00 -77.00  60.00  210
 12  \w     41.00 139.00   0.50    4.00    --  111.00 -61.00-180.00  196
 13  \w     87.00 178.00   0.50    4.00    --  111.00  30.00  60.00  182
 14  \w     87.00 178.00   0.50    4.00    --  111.00  30.00 -90.00  182
 15  \w     30.00 109.00   0.50    4.00    --  111.00 -94.00-120.00  158
 16  \w     30.00  88.00   0.50    4.00    --  111.00 -94.00  30.00  116
 17  \w     75.00 121.00   0.50    4.00    --  111.00-125.00   0.00   92
 18  \w     53.00 120.00   0.50    4.00    --  111.00-125.00  90.00  134
 19  \w     80.00 121.00   0.50    4.00    --  111.00-125.00-120.00   82
 20  \w     47.00 112.00   0.50    4.00    --  111.00 -30.00  30.00  130
 21  \w     88.00 178.00   0.50    4.00    --  111.00  45.00-150.00  180
 22  \w     40.00  80.00   0.50    4.00    --  111.00-125.00 150.00   80
 23  \w     96.00 121.00   0.50    4.00    --  111.00-125.00 150.00   50
 24  \w     98.00 135.00   0.50    4.00    --  111.00 -45.00-150.00   74
 25  \w    106.00 146.00   0.50    4.00    --  111.00  30.00 150.00   80
 26  \w     31.00  63.00   0.50    4.00    --  111.00 -94.00  90.00   64
 27  \w     48.00  89.00   0.50    4.00    --  111.00 -45.00-150.00   82
;
_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      -0.0435471000
_diffrn_orient_matrix_UB_12      0.0694555000
_diffrn_orient_matrix_UB_13      0.1145698000
_diffrn_orient_matrix_UB_21      -0.0008063000
_diffrn_orient_matrix_UB_22      0.0944143000
_diffrn_orient_matrix_UB_23      -0.1925100000
_diffrn_orient_matrix_UB_31      -0.0382852000
_diffrn_orient_matrix_UB_32      -0.0810057000
_diffrn_orient_matrix_UB_33      -0.1259143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            20567
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.045
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.145
_exptl_absorpt_correction_T_max  0.768
_exptl_absorpt_correction_T_min  0.379
_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    1.363
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.301
_exptl_crystal_size_min          0.115
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3535
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+2.5352P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                3531
_reflns_number_total             3535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           9d
_cod_database_code               1552472
_chemical_oxdiff_formula         'C76 H72 N4 P12 '
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.95(4) 0.05(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              40318
_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 1.423
_oxdiff_exptl_absorpt_empirical_full_min 0.630