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_1552469
_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         'C35 H20 N5 P5 S5, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C35.5 H21 Cl N5 P5 S5'
_chemical_formula_weight         868.17
_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             2017-07-01
_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                112.462(2)
_cell_angle_beta                 90.355(2)
_cell_angle_gamma                99.439(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2485(3)
_cell_length_b                   12.3713(3)
_cell_length_c                   15.6969(4)
_cell_measurement_reflns_used    14284
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1070
_cell_measurement_theta_min      3.9210
_cell_volume                     1809.10(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      100.00(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   -125.00  48.00   0.50    4.00    --  -38.50   0.00 -90.00  346
  2  \w    -61.00  34.00   0.50    4.00    --  -38.50  38.00 150.00  190
  3  \w     23.00  98.00   0.50    4.00    --   42.50-125.00  60.00  150
  4  \w     23.00  98.00   0.50    4.00    --   42.50-125.00-180.00  150
  5  \w      1.00  82.00   0.50    4.00    --   42.50 -99.00 -90.00  162
  6  \w     87.00 178.00   0.50   16.00    --  111.00  30.00  30.00  182
  7  \w     31.00 156.00   0.50   16.00    --  111.00 -15.00   0.00  250
  8  \w     37.00 142.00   0.50   16.00    --  111.00 -77.00-180.00  210
  9  \w     31.00 156.00   0.50   16.00    --  111.00 -15.00 120.00  250
 10  \w     39.00 121.00   0.50   16.00    --  111.00-125.00 -90.00  164
 11  \w     87.00 178.00   0.50   16.00    --  111.00  45.00-180.00  182
 12  \w     30.00 109.00   0.50   16.00    --  111.00 -94.00  90.00  158
 13  \w     39.00 121.00   0.50   16.00    --  111.00-125.00   0.00  164
 14  \w     30.00 109.00   0.50   16.00    --  111.00 -94.00 150.00  158
 15  \w     39.00 121.00   0.50   16.00    --  111.00-125.00-150.00  164
 16  \w     87.00 178.00   0.50   16.00    --  111.00  30.00 -60.00  182
 17  \w     40.00 127.00   0.50   16.00    --  111.00 -45.00 -60.00  174
 18  \w     91.00 118.00   0.50   16.00    --  111.00  61.00 120.00   54
 19  \w    140.00 177.00   0.50   16.00    --  111.00  61.00 120.00   74
 20  \w     41.00 125.00   0.50   16.00    --  111.00 -45.00-180.00  168
 21  \w     59.00 115.00   0.50   16.00    --  111.00 -61.00  60.00  112
 22  \w     41.00 109.00   0.50   16.00    --  111.00 -94.00   0.00  136
 23  \w     52.00  90.00   0.50   16.00    --  111.00-125.00  90.00   76
 24  \w     94.00 121.00   0.50   16.00    --  111.00-125.00  90.00   54
 25  \w     47.00  74.00   0.50   16.00    --  111.00 -94.00  30.00   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      0.0208520000
_diffrn_orient_matrix_UB_12      0.1366438000
_diffrn_orient_matrix_UB_13      0.0357623000
_diffrn_orient_matrix_UB_21      0.0686917000
_diffrn_orient_matrix_UB_22      -0.0039969000
_diffrn_orient_matrix_UB_23      -0.0879053000
_diffrn_orient_matrix_UB_31      -0.1349109000
_diffrn_orient_matrix_UB_32      -0.0088519000
_diffrn_orient_matrix_UB_33      -0.0483433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22889
_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         76.708
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             882
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0462P)^2^+1.6993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0883
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7164
_reflns_number_total             7537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc04501e2.cif
_cod_data_source_block           18
_cod_original_cell_volume        1809.09(8)
_cod_original_formula_sum        'C35.50 H21 Cl N5 P5 S5'
_cod_database_code               1552469
_chemical_oxdiff_formula         C35.5H20ClN5P5S5
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) C36(0.5) H36A(0.5) H36B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C28(H28),
  C32(H32), C33(H33), C34(H34), C35(H35)
;
_shelx_res_checksum              8434
_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 1.437
_oxdiff_exptl_absorpt_empirical_full_min 0.850