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_7715988
_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         'C22 H42 K O6 P3'
_chemical_formula_sum            'C22 H42 K O6 P3'
_chemical_formula_weight         534.56
_chemical_name_systematic        '[K([18]crown-6)][1,2,3-P3C2tBu2]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.58810(10)
_cell_length_b                   17.15960(10)
_cell_length_c                   17.26040(10)
_cell_measurement_reflns_used    42511
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      66.7810
_cell_measurement_theta_min      4.5500
_cell_volume                     2839.82(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -88.00 -63.00   1.00    2.00    --  -43.66 127.00   7.00   25
  2  \w    -96.00 -71.00   1.00    2.00    --  -43.66 143.00 176.00   25
  3  \w     48.00  75.00   1.00    2.00    --   43.66-143.00 121.00   27
  4  \w     28.00  55.00   1.00    2.00    --   43.66-127.00 -68.00   27
  5  \w     67.00  92.00   1.00    2.00    --   43.66 143.00 176.00   25
  6  \w     92.00 117.00   1.00    8.00    --   86.50 127.00   7.00   25
  7  \w     33.00  58.00   1.00    8.00    --   86.50-143.00 121.00   25
  8  \w     26.00  51.00   1.00    8.00    --   86.50-127.00 -68.00   25
  9  \w   -154.00-129.00   1.00    8.00    --  -90.00-127.00 -68.00   25
 10  \w   -149.00-124.00   1.00    8.00    --  -90.00-143.00 121.00   25
 11  \w   -105.00 -80.00   1.00    8.00    --  -90.00 143.00 176.00   25
 12  \w    -97.00 -71.00   1.00    8.00    --  -90.00 127.00   7.00   26
 13  \w    -77.00 -49.00   1.00    2.00    --  -43.66 125.00-180.00   28
 14  \w    -94.00 -43.00   1.00    2.00    --  -43.66 125.00-120.00   51
 15  \w     18.00 113.00   1.00    2.00    --   43.66  57.00  60.00   95
 16  \w     20.00 112.00   1.00    2.00    --   43.66  57.00-180.00   92
 17  \w     44.00 113.00   1.00    2.00    --   43.66  57.00 -60.00   69
 18  \w   -153.00-114.00   1.00    8.00    --  -90.00 -61.00-180.00   39
 19  \w    -59.00 -29.00   1.00    8.00    --  -90.00  77.00   0.00   30
 20  \w    -61.00 -36.00   1.00    8.00    --  -90.00 125.00 -30.00   25
 21  \w    -46.00 -19.00   1.00    8.00    --  -90.00 109.00-123.93   27
 22  \w    -69.00 -44.00   1.00    8.00    --  -90.00 125.00 120.00   25
 23  \w    -48.00 -21.00   1.00    8.00    --  -90.00  77.00  30.00   27
 24  \w   -153.00-107.00   1.00    8.00    --  -90.00 -77.00  60.00   46
 25  \w   -163.00-119.00   1.00    8.00    --  -90.00 -94.00  90.00   44
 26  \w    -75.00 -47.00   1.00    8.00    --  -90.00  97.00  92.22   28
 27  \w   -112.00 -70.00   1.00    8.00    --  -90.00 125.00 -30.00   42
 28  \w   -110.00 -72.00   1.00    8.00    --  -90.00 125.00 120.00   38
 29  \w   -158.00-131.00   1.00    8.00    --  -90.00-125.00 -60.00   27
 30  \w    -98.00 -67.00   1.00    8.00    --  -90.00 -51.00  -5.69   31
 31  \w   -167.00-117.00   1.00    8.00    --  -90.00 -15.00 -60.00   50
 32  \w   -108.00 -60.00   1.00    8.00    --  -90.00 109.00-123.93   48
 33  \w   -161.00-106.00   1.00    8.00    --  -90.00-125.00   0.00   55
 34  \w   -100.00 -73.00   1.00    8.00    --  -90.00  77.00  30.00   27
 35  \w   -106.00 -69.00   1.00    8.00    --  -90.00 125.00-120.00   37
 36  \w    -95.00 -16.00   1.00    8.00    --  -90.00  77.00-120.00   79
 37  \w    -96.00 -71.00   1.00    8.00    --  -90.00 125.00  30.00   25
 38  \w   -111.00 -56.00   1.00    8.00    --  -90.00 125.00  60.00   55
 39  \w   -161.00-117.00   1.00    8.00    --  -90.00 -15.00 150.00   44
 40  \w    -76.00 -51.00   1.00    8.00    --  -90.00 -15.00 150.00   25
 41  \w    -74.00 -21.00   1.00    8.00    --  -90.00  45.00-150.00   53
 42  \w   -105.00 -74.00   1.00    8.00    --  -90.00  30.00  60.00   31
 43  \w   -113.00 -25.00   1.00    8.00    --  -90.00  45.00  90.00   88
 44  \w    -92.00 -64.00   1.00    8.00    --  -90.00 113.00   4.30   28
 45  \w   -107.00 -67.00   1.00    8.00    --  -90.00  45.00 -30.00   40
 46  \w   -158.00-133.00   1.00    8.00    --  -90.00-125.00 -30.00   25
 47  \w   -121.00 -93.00   1.00    8.00    --  -90.00 -61.00 -30.00   28
 48  \w   -157.00-115.00   1.00    8.00    --  -90.00 -61.00 120.00   42
 49  \w    -98.00 -71.00   1.00    8.00    --  -90.00 -61.00 120.00   27
 50  \w   -128.00 -66.00   1.00    8.00    --  -90.00  15.00-180.00   62
 51  \w    -49.00 -22.00   1.00    8.00    --  -90.00  30.00  60.00   27
 52  \w   -163.00-138.00   1.00    8.00    --  -90.00 -77.00 -30.00   25
 53  \w   -134.00-109.00   1.00    8.00    --  -90.00-125.00-180.00   25
 54  \w   -133.00-108.00   1.00    8.00    --  -90.00-125.00-150.00   25
 55  \w   -127.00 -54.00   1.00    8.00    --  -90.00 145.00-129.06   73
 56  \w    -99.00 -64.00   1.00    8.00    --  -90.00 -61.00-180.00   35
 57  \w    -94.00 -46.00   1.00    8.00    --  -90.00 125.00  90.00   48
 58  \w    -84.00 -59.00   1.00    8.00    --  -90.00 125.00-180.00   25
 59  \w    -54.00 -27.00   1.00    8.00    --  -90.00  61.00-150.00   27
 60  \w    -94.00 -66.00   1.00    8.00    --  -90.00 125.00 -60.00   28
 61  \w    -53.00 -28.00   1.00    8.00    --  -90.00 125.00 -60.00   25
 62  \w   -110.00 -83.00   1.00    8.00    --  -90.00 116.00  65.02   27
 63  \w   -106.00 -81.00   1.00    8.00    --  -90.00  50.00 115.08   25
 64  \w    -94.00 -69.00   1.00    8.00    --  -90.00  39.00-118.09   25
 65  \w    -75.00 -48.00   1.00    8.00    --  -90.00  39.00  18.24   27
 66  \w    -87.00 -60.00   1.00    8.00    --  -90.00  61.00-120.00   27
 67  \w    -63.00 -28.00   1.00    8.00    --  -90.00  30.00 150.00   35
 68  \w    -81.00 -56.00   1.00    8.00    --  -90.00  77.00 -90.00   25
 69  \w   -106.00 -81.00   1.00    8.00    --  -90.00  82.00 149.49   25
 70  \w   -162.00-126.00   1.00    8.00    --  -90.00 -15.00 -30.00   36
 71  \w    -67.00 -22.00   1.00    8.00    --  -90.00   0.00 -30.00   45
 72  \w   -145.00-104.00   1.00    8.00    --  -90.00 -77.00-150.00   41
;
_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      0.0821941000
_diffrn_orient_matrix_UB_12      0.0768822000
_diffrn_orient_matrix_UB_13      0.0065037000
_diffrn_orient_matrix_UB_21      0.1330327000
_diffrn_orient_matrix_UB_22      -0.0461002000
_diffrn_orient_matrix_UB_23      0.0200830000
_diffrn_orient_matrix_UB_31      0.0369319000
_diffrn_orient_matrix_UB_32      -0.0050215000
_diffrn_orient_matrix_UB_33      -0.0867146000
_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  0.0493
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.826
_diffrn_reflns_theta_max         66.826
_diffrn_reflns_theta_min         3.632
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.503
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.91a (Rigaku Oxford Diffraction, 2020)
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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane/toluene'
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.253
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 2132 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0409P)^2^+0.4491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0634
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4990
_reflns_number_total             5040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01067a2.cif
_cod_data_source_block           mu025_tp
_cod_depositor_comments
'Adding full bibliography for 7715982--7715988.cif.'
_cod_database_code               7715988
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C22H42KO6P3
_chemical_oxdiff_usercomment     'crystals from toluene nhex'
_reflns_odcompleteness_completeness 98.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.46
_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:
 C14(H14A,H14B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B), C22(H22A,
 H22B), C11(H11A,H11B), C19(H19A,H19B), C16(H16A,H16B), C12(H12A,H12B),
 C20(H20A,H20B), C21(H21A,H21B), C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C10(H10A,
 H10B,H10C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              65356
_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 2.372
_oxdiff_exptl_absorpt_empirical_full_min 0.548