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_7715983
_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 O6 P3 Rb'
_chemical_formula_sum            'C22 H42 O6 P3 Rb'
_chemical_formula_weight         580.93
_chemical_name_systematic        '[Rb([18]crown-6)][1,2,3-P3C2tBu2]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 106.4890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.31930(10)
_cell_length_b                   16.00110(10)
_cell_length_c                   17.6998(2)
_cell_measurement_reflns_used    32419
_cell_measurement_temperature    123.05(10)
_cell_measurement_theta_max      66.7080
_cell_measurement_theta_min      4.4670
_cell_volume                     2802.40(5)
_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      123.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     75.00 112.00   1.00    1.72    --   43.43  66.00  78.00   37
  2  \w     47.00  72.00   1.00    1.72    --   43.43  66.00  78.00   25
  3  \w    -27.00  71.00   1.00    1.72    --   43.43 -66.00 -56.00   98
  4  \w     41.00  66.00   1.00    6.86    --   86.50 -66.00 -56.00   25
  5  \w     83.00 108.00   1.00    6.86    --   86.50  66.00  78.00   25
  6  \w   -103.00 -75.00   1.00    6.86    --  -90.00  66.00  78.00   28
  7  \w   -145.00-118.00   1.00    6.86    --  -90.00 -66.00 -56.00   27
  8  \w    -62.00 -35.00   1.00    6.86    --  -90.00  66.00  78.00   27
  9  \w    -41.00  27.00   1.00    1.72    --  -43.43  66.00  78.00   68
 10  \w   -100.00 -73.00   1.00    1.72    --  -43.43 -66.00 -56.00   27
 11  \w      9.00  84.00   1.00    1.72    --   43.43-125.00-180.00   75
 12  \w     85.00 129.00   1.00    6.86    --   86.50  77.00   0.00   44
 13  \w   -106.00 -27.00   1.00    6.86    --  -90.00 125.00 120.00   79
 14  \w   -111.00 -79.00   1.00    6.86    --  -90.00 125.00  60.00   32
 15  \w   -108.00 -74.00   1.00    6.86    --  -90.00 125.00-150.00   34
 16  \w   -172.00-147.00   1.00    6.86    --  -90.00 -94.00  90.00   25
 17  \w   -154.00-110.00   1.00    6.86    --  -90.00 -77.00   0.00   44
 18  \w   -133.00-104.00   1.00    6.86    --  -90.00 -94.00  90.00   29
 19  \w   -142.00 -97.00   1.00    6.86    --  -90.00-125.00 -90.00   45
 20  \w    -96.00 -27.00   1.00    6.86    --  -90.00 125.00 -90.00   69
 21  \w   -111.00 -86.00   1.00    6.86    --  -90.00  45.00  90.00   25
 22  \w    -73.00 -22.00   1.00    6.86    --  -90.00  45.00  90.00   51
 23  \w   -113.00 -46.00   1.00    6.86    --  -90.00  61.00-180.00   67
 24  \w   -144.00-117.00   1.00    6.86    --  -90.00 -77.00-150.00   27
 25  \w   -161.00-101.00   1.00    6.86    --  -90.00-125.00 120.00   60
 26  \w   -111.00 -86.00   1.00    6.86    --  -90.00 125.00 -30.00   25
 27  \w    -72.00 -27.00   1.00    6.86    --  -90.00 125.00 -30.00   45
 28  \w    -61.00 -27.00   1.00    6.86    --  -90.00  30.00 -90.00   34
 29  \w   -120.00 -85.00   1.00    6.86    --  -90.00  77.00  90.00   35
 30  \w    -50.00 -21.00   1.00    6.86    --  -90.00  77.00  90.00   29
 31  \w    -52.00 -27.00   1.00    6.86    --  -90.00 125.00 -60.00   25
 32  \w   -147.00-120.00   1.00    6.86    --  -90.00 -30.00 -60.00   27
 33  \w   -109.00 -63.00   1.00    6.86    --  -90.00 -30.00 -60.00   46
 34  \w   -112.00 -82.00   1.00    6.86    --  -90.00 125.00 -60.00   30
 35  \w    -98.00 -71.00   1.00    6.86    --  -90.00  77.00 -30.00   27
 36  \w    -41.00 -16.00   1.00    6.86    --  -90.00  77.00 -30.00   25
 37  \w    -95.00 -53.00   1.00    6.86    --  -90.00 125.00  90.00   42
 38  \w    -75.00 -27.00   1.00    6.86    --  -90.00 125.00 150.00   48
 39  \w   -109.00 -83.00   1.00    6.86    --  -90.00 125.00   0.00   26
 40  \w    -68.00 -36.00   1.00    6.86    --  -90.00 125.00  60.00   32
 41  \w   -126.00 -96.00   1.00    6.86    --  -90.00  15.00-150.00   30
 42  \w    -71.00 -12.00   1.00    6.86    --  -90.00  15.00-150.00   59
 43  \w    -99.00 -72.00   1.00    6.86    --  -90.00  45.00  60.00   27
 44  \w    -57.00 -28.00   1.00    6.86    --  -90.00  45.00  60.00   29
 45  \w   -105.00 -65.00   1.00    6.86    --  -90.00  77.00 120.00   40
 46  \w   -112.00 -47.00   1.00    6.86    --  -90.00 125.00-180.00   65
 47  \w   -117.00 -73.00   1.00    6.86    --  -90.00  30.00-120.00   44
 48  \w    -61.00 -18.00   1.00    6.86    --  -90.00  30.00-120.00   43
 49  \w   -100.00 -29.00   1.00    6.86    --  -90.00 125.00-120.00   71
 50  \w   -114.00 -61.00   1.00    6.86    --  -90.00  45.00   0.00   53
 51  \w   -160.00 -94.00   1.00    6.86    --  -90.00 -45.00 120.00   66
 52  \w   -119.00 -94.00   1.00    6.86    --  -90.00  77.00 -90.00   25
 53  \w    -69.00 -29.00   1.00    6.86    --  -90.00  77.00 -90.00   40
 54  \w   -157.00-130.00   1.00    6.86    --  -90.00-125.00  60.00   27
 55  \w    -54.00 -27.00   1.00    6.86    --  -90.00 125.00-150.00   27
;
_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      -0.1317878000
_diffrn_orient_matrix_UB_12      -0.0078170000
_diffrn_orient_matrix_UB_13      -0.0675868000
_diffrn_orient_matrix_UB_21      0.0358275000
_diffrn_orient_matrix_UB_22      -0.0911653000
_diffrn_orient_matrix_UB_23      -0.0135527000
_diffrn_orient_matrix_UB_31      -0.0747072000
_diffrn_orient_matrix_UB_32      -0.0299698000
_diffrn_orient_matrix_UB_33      0.0590665000
_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  0.0518
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            42970
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.781
_diffrn_reflns_theta_max         66.781
_diffrn_reflns_theta_min         4.488
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.320
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.254
_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 orangish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane/THF'
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.192
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0574P)^2^+7.0094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1148
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4855
_reflns_number_total             4954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01067a2.cif
_cod_data_source_block           mu297_mp
_cod_depositor_comments
'Adding full bibliography for 7715982--7715988.cif.'
_cod_database_code               7715983
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C22 H42 O6 P3 Rb1 '
_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. Rigid body (RIGU) restrains
 C19, O5, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C17(H17A,H17B), C18(H18A,H18B), C13(H13A,H13B), C11(H11A,
 H11B), C22(H22A,H22B), C21(H21A,H21B), C16(H16A,H16B), C15(H15A,H15B),
 C12(H12A,H12B), C14(H14A,H14B), C20(H20A,H20B)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C5(H5A,
 H5B,H5C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              12269
_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 1.706
_oxdiff_exptl_absorpt_empirical_full_min 0.714