Access to 1,2,3-triphospholide ligands by reduction of di-<i>tert</i>-butyldiphosphatetrahedrane.
Uttendorfer, Maria K.; Hierlmeier, Gabriele; Balázs, Gábor; Wolf, Robert; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10113–10119; doi:10.1039/d4dt01067a

data_7715987
_publ_section_title
;
 Access to 1,2,3-triphospholide ligands by reduction of
 di-<i>tert</i>-butyldiphosphatetrahedrane.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10113
_journal_page_last               10119
_journal_paper_doi               10.1039/d4dt01067a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C20 H36 P6'
_chemical_formula_sum            'C20 H36 P6'
_chemical_formula_weight         462.31
_chemical_name_systematic        tBu4C4P6
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-04
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.755(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2177(5)
_cell_length_b                   12.5176(3)
_cell_length_c                   22.1442(6)
_cell_measurement_reflns_used    8453
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.7690
_cell_measurement_theta_min      4.3280
_cell_volume                     4912.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 42.92a 64-bit (release 29-05-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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     34.00  59.00   0.50    1.42    --   62.92  15.00 -30.00   50
  2  \w     28.00  57.00   0.50    1.42    --   62.92 -95.00  90.00   58
  3  \w     68.00 107.00   0.50    1.42    --   62.92  15.00 -30.00   78
  4  \w     26.00  68.00   0.50    1.42    --   62.92 -95.00-150.00   84
  5  \w     26.00  51.00   0.50    1.42    --   62.92 -95.00  60.00   50
  6  \w    -60.00 -25.00   0.50    1.42    --  -63.82 125.00 -60.00   70
  7  \w   -106.00 -70.00   0.50    1.42    --  -63.82 -15.00 150.00   72
  8  \w    -74.00 -24.00   0.50    1.42    --  -63.82 125.00  90.00  100
  9  \w    -97.00 -54.00   0.50    1.42    --  -73.68 125.00-180.00   86
 10  \w   -100.00 -68.00   0.50    1.42    --  -73.68 125.00  60.00   64
 11  \w   -117.00 -47.00   0.50    1.42    --  -73.68 -15.00-120.00  140
 12  \w   -110.00 -40.00   0.50    1.42    --  -73.68   0.00 -30.00  140
 13  \w   -100.00 -38.00   0.50    1.42    --  -73.68 125.00 -90.00  124
 14  \w     42.00  68.00   0.50    1.42    --   75.56 -95.00-120.00   52
 15  \w     40.00  65.00   0.50    1.42    --   75.87 -95.00 150.00   50
 16  \w     42.00  68.00   0.50    1.42    --   75.87 -95.00-180.00   52
 17  \w     52.00  77.00   0.50    1.42    --   75.87  15.00 -30.00   50
 18  \w    -73.00 -46.00   0.50    1.42    --  -76.65 -15.00  90.00   54
 19  \w   -114.00 -88.00   0.50    1.42    --  -78.25-172.00 -55.85   52
 20  \w   -111.00 -80.00   0.50    1.42    --  -78.25 -86.00-149.68   62
 21  \w    -69.00 -43.00   0.50    1.42    --  -78.25  89.00  58.97   52
 22  \w   -112.00 -76.00   0.50    1.42    --  -78.25 135.00  -7.59   72
 23  \w    -64.00 -37.00   0.50    1.42    --  -78.25 120.00  61.17   54
 24  \w    -88.00 -62.00   0.50    1.42    --  -78.25 121.00 -35.80   52
 25  \w   -103.00 -77.00   0.50    1.42    --  -78.25 140.00 147.91   52
 26  \w   -112.00 -86.00   0.50    1.42    --  -78.25 135.00-151.69   52
 27  \w    -92.00 -66.00   0.50    1.42    --  -78.25 115.00 168.52   52
 28  \w    -74.00 -48.00   0.50    1.42    --  -78.25 125.00 -90.85   52
 29  \w   -112.00 -81.00   0.50    1.42    --  -78.25 135.00-177.57   62
 30  \w    -67.00 -40.00   0.50    1.42    --  -78.25 135.00-177.57   54
 31  \w   -103.00 -58.00   0.50    1.42    --  -78.25 122.00 136.84   90
 32  \w   -112.00 -87.00   0.50    1.42    --  -78.25 -33.00 -26.81   50
 33  \w   -102.00 -74.00   0.50    1.42    --  -78.25 120.00  61.17   56
 34  \w    -66.00 -38.00   0.50    1.42    --  -78.25 110.00-144.96   56
 35  \w   -113.00 -62.00   0.50    1.42    --  -78.25 137.00 -75.36  102
 36  \w    -89.00 -41.00   0.50    1.42    --  -78.25 118.00-137.77   96
 37  \w   -100.00 -51.00   0.50    1.42    --  -78.25 116.00  55.86   98
 38  \w   -108.00 -82.00   0.50    1.42    --  -78.25 131.00  67.58   52
 39  \w   -104.00 -59.00   0.50    1.42    --  -78.25 123.00 104.06   90
 40  \w   -105.00 -80.00   0.50    1.42    --  -78.25 125.00 -90.85   50
 41  \w    -80.00 -45.00   0.50    1.42    --  -78.25-172.00 -55.85   70
 42  \w     59.00 125.00   0.50    1.42    --   79.75  19.00-151.64  132
 43  \w     40.00  68.00   0.50    1.42    --   79.75 -64.00  -4.88   56
 44  \w     58.00 101.00   0.50    1.42    --   79.75  20.00  -0.26   86
 45  \w     91.00 123.00   0.50    1.42    --   79.75  21.00  78.60   64
 46  \w     65.00 101.00   0.50    1.42    --   79.75  22.00  51.17   72
 47  \w     65.00 111.00   0.50    1.42    --   79.75  22.00 136.70   92
 48  \w     40.00  70.00   0.50    1.42    --   79.75  -4.00 -52.45   60
 49  \w     44.00 110.00   0.50    1.42    --   79.75   0.00 162.79  132
 50  \w     56.00  86.00   0.50    1.42    --   79.75-111.00 -43.15   60
 51  \w     47.00  83.00   0.50    1.42    --   79.75  -4.00-129.61   72
 52  \w     71.00 109.00   0.50    1.42    --   79.75-128.00  76.96   76
 53  \w     43.00  68.00   0.50    1.42    --   79.75-128.00  76.96   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0545368000
_diffrn_orient_matrix_UB_12      0.0803719000
_diffrn_orient_matrix_UB_13      -0.0478477000
_diffrn_orient_matrix_UB_21      0.0533296000
_diffrn_orient_matrix_UB_22      0.0097412000
_diffrn_orient_matrix_UB_23      -0.0367604000
_diffrn_orient_matrix_UB_31      -0.0416706000
_diffrn_orient_matrix_UB_32      -0.0926615000
_diffrn_orient_matrix_UB_33      -0.0453337000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.400
_diffrn_reflns_theta_min         4.324
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.088
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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 brownish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.029
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5007
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0734P)^2^+4.2853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1174
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4366
_reflns_number_total             5007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01067a2.cif
_cod_data_source_block           mu321_2_mc
_cod_depositor_comments
'Adding full bibliography for 7715982--7715988.cif.'
_cod_database_code               7715987
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H36 P6'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C6(H6A,H6B,H6C),
 C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
  C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C12(H12A,H12B,
 H12C)
;
_shelx_res_checksum              30566
_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 1.239
_oxdiff_exptl_absorpt_empirical_full_min 0.756