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_7715986
_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         'C27 H51 O6 P2 Rb'
_chemical_formula_sum            'C27 H51 O6 P2 Rb'
_chemical_formula_weight         619.08
_chemical_name_systematic        '[Rb([18]crown-6)][1,3-P2C3tBu3]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                90.511(2)
_cell_angle_beta                 98.341(2)
_cell_angle_gamma                101.542(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3862(2)
_cell_length_b                   10.5727(2)
_cell_length_c                   16.3426(4)
_cell_measurement_reflns_used    34160
_cell_measurement_temperature    123.02(10)
_cell_measurement_theta_max      66.8190
_cell_measurement_theta_min      4.7860
_cell_volume                     1570.99(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 42.90a 64-bit (release 14-04-2023))'
_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      123.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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   -116.00 -89.00   1.00    2.00    --  -43.68 -13.00-166.00   27
  2  \w     81.00 115.00   1.00    2.00    --   43.68  13.00   5.00   34
  3  \w    -35.00  85.00   1.00    2.00    --   43.68 -13.00-166.00  120
  4  \w     24.00  59.00   1.00    2.00    --   43.68  13.00   5.00   35
  5  \w     77.00 102.00   1.00    7.00    --   86.50  13.00   5.00   25
  6  \w     44.00  69.00   1.00    7.00    --   86.50 -13.00-166.00   25
  7  \w   -166.00-134.00   1.00    7.00    --  -90.00 -13.00-166.00   32
  8  \w   -108.00 -63.00   1.00    7.00    --  -90.00 -13.00-166.00   45
  9  \w     -6.00  21.00   1.00    2.00    --   26.00  81.00 148.59   27
 10  \w      5.00  32.00   1.00    2.00    --  -43.68  13.00   5.00   27
 11  \w    -40.00  -3.00   1.00    2.00    --  -43.68 -13.00-166.00   37
 12  \w    -49.00 -24.00   1.00    2.00    --  -43.68  13.00   5.00   25
 13  \w    -94.00 -37.00   1.00    2.00    --  -43.68 125.00  60.00   57
 14  \w     19.00  56.00   1.00    2.00    --   43.68  37.00  60.00   37
 15  \w      7.00  85.00   1.00    2.00    --   43.68-125.00-180.00   78
 16  \w     21.00  55.00   1.00    2.00    --   50.00  69.00 -12.05   34
 17  \w     67.00 110.00   1.00    2.00    --   50.00  71.00-165.57   43
 18  \w     21.00  69.00   1.00    2.00    --   50.00  69.00 -73.37   48
 19  \w     20.00  62.00   1.00    2.00    --   50.00  71.00-165.57   42
 20  \w     60.00  91.00   1.00    2.00    --   50.00  69.00 -12.05   31
 21  \w     64.00  91.00   1.00    2.00    --   54.00  71.00  49.48   27
 22  \w     26.00  55.00   1.00    2.00    --   54.00  71.00  49.48   29
 23  \w     28.00  55.00   1.00    2.00    --   58.00  71.00  98.96   27
 24  \w     34.00  78.00   1.00    2.00    --   62.00  71.00 143.70   44
 25  \w     34.00  67.00   1.00    2.00    --   62.00  71.00 120.33   33
 26  \w     34.00  63.00   1.00    2.00    --   62.00  69.00  65.89   29
 27  \w     98.00 126.00   1.00    2.00    --   62.00  71.00 143.70   28
 28  \w     33.00 103.00   1.00    2.00    --   62.00  70.00-148.13   70
 29  \w     32.00  81.00   1.00    2.00    --   62.00  71.00   1.87   49
 30  \w     38.00  64.00   1.00    2.00    --   66.00  70.00-108.56   26
 31  \w     37.00  64.00   1.00    2.00    --   66.00  70.00 177.48   27
 32  \w     37.00  64.00   1.00    2.00    --   66.00  71.00 -57.21   27
 33  \w     41.00  67.00   1.00    7.00    --   70.00  70.00 -81.28   26
 34  \w     44.00  70.00   1.00    7.00    --   74.00  71.00  21.96   26
 35  \w   -159.00 -63.00   1.00    7.00    --  -90.00 -61.00 130.71   96
 36  \w   -142.00 -61.00   1.00    7.00    --  -90.00 -70.00 -79.56   81
 37  \w   -159.00-131.00   1.00    7.00    --  -90.00 -65.00-119.48   28
 38  \w    -97.00 -63.00   1.00    7.00    --  -90.00 -64.00 -77.22   34
 39  \w   -111.00 -44.00   1.00    7.00    --  -90.00 125.00-150.00   67
 40  \w   -161.00-102.00   1.00    7.00    --  -90.00-125.00  60.00   59
 41  \w    -88.00 -61.00   1.00    7.00    --  -90.00 -67.00 -24.86   27
 42  \w   -159.00-108.00   1.00    7.00    --  -90.00 -67.00 -24.86   51
 43  \w    -89.00 -62.00   1.00    7.00    --  -90.00 -66.00   0.12   27
 44  \w   -133.00 -64.00   1.00    7.00    --  -90.00 -68.00-125.66   69
 45  \w    -85.00 -60.00   1.00    7.00    --  -90.00 -71.00 171.03   25
 46  \w   -153.00 -96.00   1.00    7.00    --  -90.00 -66.00   0.12   57
 47  \w    -75.00 -17.00   1.00    7.00    --  -90.00  77.00  30.00   58
 48  \w    -52.00 -27.00   1.00    7.00    --  -90.00  13.00   5.00   25
 49  \w   -149.00-115.00   1.00    7.00    --  -90.00 -71.00 171.03   34
 50  \w   -161.00-131.00   1.00    7.00    --  -90.00-125.00 -60.00   30
 51  \w   -102.00 -62.00   1.00    7.00    --  -90.00 -64.00 145.97   40
 52  \w   -157.00-122.00   1.00    7.00    --  -90.00 -64.00 145.97   35
 53  \w   -112.00 -38.00   1.00    7.00    --  -90.00 125.00 -60.00   74
 54  \w   -148.00-111.00   1.00    7.00    --  -90.00 -69.00-141.10   37
 55  \w    -90.00 -62.00   1.00    7.00    --  -90.00 -69.00-141.10   28
 56  \w   -161.00-117.00   1.00    7.00    --  -90.00 -68.00 -38.29   44
 57  \w    -99.00 -61.00   1.00    7.00    --  -90.00 -68.00 -38.29   38
 58  \w    -97.00 -53.00   1.00    7.00    --  -90.00  77.00 -60.00   44
 59  \w   -113.00 -88.00   1.00    7.00    --  -90.00  45.00 -60.00   25
 60  \w    -73.00 -32.00   1.00    7.00    --  -90.00  45.00 -60.00   41
 61  \w   -141.00 -61.00   1.00    7.00    --  -90.00 -68.00  26.54   80
 62  \w    -89.00 -60.00   1.00    7.00    --  -90.00 -71.00  78.48   29
 63  \w   -121.00 -70.00   1.00    7.00    --  -90.00  77.00-120.00   51
 64  \w    -99.00 -66.00   1.00    7.00    --  -90.00 -65.00-119.48   33
 65  \w   -153.00-104.00   1.00    7.00    --  -90.00 -71.00  78.48   49
 66  \w   -114.00 -19.00   1.00    7.00    --  -90.00  45.00  30.00   95
 67  \w   -101.00 -61.00   1.00    7.00    --  -90.00 -67.00  60.81   40
 68  \w   -109.00 -61.00   1.00    7.00    --  -90.00 -70.00 -51.59   48
 69  \w   -105.00 -70.00   1.00    7.00    --  -90.00 104.00  54.94   35
 70  \w    -48.00 -12.00   1.00    7.00    --  -90.00 104.00  54.94   36
 71  \w    -86.00 -61.00   1.00    7.00    --  -90.00 -67.00  93.50   25
 72  \w    -54.00 -27.00   1.00    7.00    --  -90.00  61.00-180.00   27
 73  \w   -114.00 -66.00   1.00    7.00    --  -90.00  61.00-180.00   48
 74  \w    -88.00 -61.00   1.00    7.00    --  -90.00 -68.00 107.51   27
 75  \w   -159.00 -61.00   1.00    7.00    --  -90.00 -70.00  53.84   98
 76  \w   -131.00-104.00   1.00    7.00    --  -90.00 -67.00  60.81   27
 77  \w   -152.00 -91.00   1.00    7.00    --  -90.00 -68.00 107.51   61
 78  \w    -87.00 -62.00   1.00    7.00    --  -90.00 -65.00  79.80   25
 79  \w    -87.00 -61.00   1.00    7.00    --  -90.00 -68.00-177.69   26
 80  \w   -107.00 -64.00   1.00    7.00    --  -90.00 -59.00 -23.38   43
 81  \w   -151.00-124.00   1.00    7.00    --  -90.00 -59.00 -23.38   27
 82  \w   -127.00-100.00   1.00    7.00    --  -90.00 -67.00  93.50   27
 83  \w   -158.00 -97.00   1.00    7.00    --  -90.00 -68.00-177.69   61
 84  \w    -96.00 -69.00   1.00    7.00    --  -90.00 125.00 120.00   27
 85  \w   -148.00 -60.00   1.00    7.00    --  -90.00 -71.00 -93.85   88
 86  \w   -112.00 -45.00   1.00    7.00    --  -90.00 125.00-180.00   67
 87  \w    -86.00 -61.00   1.00    7.00    --  -90.00 -71.00 137.75   25
 88  \w   -111.00 -66.00   1.00    7.00    --  -90.00 125.00  60.00   45
 89  \w    -76.00 -19.00   1.00    7.00    --  -90.00  45.00-180.00   57
 90  \w   -125.00 -62.00   1.00    7.00    --  -90.00 -66.00-165.37   63
 91  \w   -120.00 -93.00   1.00    7.00    --  -90.00  84.00  41.78   27
 92  \w    -66.00 -14.00   1.00    7.00    --  -90.00  84.00  41.78   52
 93  \w   -116.00 -76.00   1.00    7.00    --  -90.00  13.00   5.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1605872000
_diffrn_orient_matrix_UB_12      0.0152624000
_diffrn_orient_matrix_UB_13      -0.0035845000
_diffrn_orient_matrix_UB_21      -0.0464030000
_diffrn_orient_matrix_UB_22      -0.1446639000
_diffrn_orient_matrix_UB_23      0.0162098000
_diffrn_orient_matrix_UB_31      0.0276712000
_diffrn_orient_matrix_UB_32      0.0314744000
_diffrn_orient_matrix_UB_33      0.0938915000
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42737
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.690
_diffrn_reflns_theta_max         66.690
_diffrn_reflns_theta_min         4.271
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.418
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.542
_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 bluish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane/THF'
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0244P)^2^+7.0505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1230
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5447
_reflns_number_total             5528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01067a2.cif
_cod_data_source_block           mu297_diphos
_cod_depositor_comments
'Adding full bibliography for 7715982--7715988.cif.'
_cod_database_code               7715986
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C27 H51 O6 P2 Rb1 '
_shelx_estimated_absorpt_t_max   0.594
_shelx_estimated_absorpt_t_min   0.459
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C17(H17A,H17B), C23(H23A,H23B), C19(H19A,H19B), C21(H21A,
 H21B), C24(H24A,H24B), C20(H20A,H20B), C16(H16A,H16B), C22(H22A,H22B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C),
 C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C),
  C11(H11A,H11B,H11C)
;
_shelx_res_checksum              25301
_olex2_date_sample_data_collection 2023-05-05
_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 1.843
_oxdiff_exptl_absorpt_empirical_full_min 0.760