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_7715985
_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 H33 Fe P3'
_chemical_formula_sum            'C20 H33 Fe P3'
_chemical_formula_weight         422.22
_chemical_name_systematic        '[Cp*Fe(?5-1,2,3-P3C2tBu2)]'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-05
_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                 107.870(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1779(2)
_cell_length_b                   12.7916(2)
_cell_length_c                   16.4260(2)
_cell_measurement_reflns_used    8850
_cell_measurement_temperature    122.97(16)
_cell_measurement_theta_max      66.6000
_cell_measurement_theta_min      4.4480
_cell_volume                     2035.35(6)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 41.109a 64-bit (release 07-05-2021))'
_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      122.97(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_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    -45.00 -20.00   1.00    4.00    --  -43.66  47.00-135.00   25
  2  \w     35.00 108.00   1.00    4.00    --   43.66  47.00-135.00   73
  3  \w     19.00  49.00   1.00    4.00    --   43.66 -47.00  75.00   30
  4  \w     85.00 110.00   1.00   14.00    --   86.50  47.00-135.00   25
  5  \w     39.00  64.00   1.00   14.00    --   86.50 -47.00  75.00   25
  6  \w    -80.00 -54.00   1.00   14.00    --  -90.00  47.00-135.00   26
  7  \w   -137.00-112.00   1.00   14.00    --  -90.00 -47.00  75.00   25
  8  \w    -95.00 -21.00   1.00    4.00    --  -43.66 -37.00 -90.00   74
  9  \w    -63.00 -27.00   1.00    4.00    --  -43.66 125.00 -30.00   36
 10  \w    -53.00 -28.00   1.00   14.00    --  -90.00  61.00 150.00   25
 11  \w   -104.00 -75.00   1.00   14.00    --  -90.00  61.00 150.00   29
 12  \w   -163.00 -63.00   1.00   14.00    --  -90.00 -29.00 127.50  100
 13  \w   -142.00-116.00   1.00   14.00    --  -90.00-125.00-150.00   26
 14  \w   -172.00-107.00   1.00   14.00    --  -90.00 -94.00 -60.00   65
 15  \w   -142.00-116.00   1.00   14.00    --  -90.00 -73.00 163.59   26
 16  \w   -163.00-137.00   1.00   14.00    --  -90.00 -77.00 150.00   26
 17  \w   -151.00-126.00   1.00   14.00    --  -90.00 -77.00  90.00   25
 18  \w   -161.00-113.00   1.00   14.00    --  -90.00-125.00-180.00   48
 19  \w   -103.00 -46.00   1.00   14.00    --  -90.00  30.00 120.00   57
 20  \w   -103.00 -77.00   1.00   14.00    --  -90.00 125.00 -60.00   26
 21  \w   -158.00-133.00   1.00   14.00    --  -90.00 -77.00-180.00   25
 22  \w    -87.00 -62.00   1.00   14.00    --  -90.00  27.00  34.94   25
 23  \w   -117.00 -91.00   1.00   14.00    --  -90.00  77.00  60.00   26
 24  \w   -112.00 -37.00   1.00   14.00    --  -90.00 125.00 -30.00   75
;
_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      -0.0600775000
_diffrn_orient_matrix_UB_12      0.0788593000
_diffrn_orient_matrix_UB_13      0.0499646000
_diffrn_orient_matrix_UB_21      -0.1393607000
_diffrn_orient_matrix_UB_22      -0.0580323000
_diffrn_orient_matrix_UB_23      -0.0287374000
_diffrn_orient_matrix_UB_31      0.0476189000
_diffrn_orient_matrix_UB_32      -0.0701360000
_diffrn_orient_matrix_UB_33      0.0799072000
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12907
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        66.789
_diffrn_reflns_theta_max         66.789
_diffrn_reflns_theta_min         4.466
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.148
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.639
_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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00062(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0280
_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^)+(0.0459P)^2^+0.8853P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3371
_reflns_number_total             3510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01067a2.cif
_cod_data_source_block           mu113_mc
_cod_depositor_comments
'Adding full bibliography for 7715982--7715988.cif.'
_cod_database_code               7715985
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H33 P3 Fe '
_shelx_estimated_absorpt_t_max   0.417
_shelx_estimated_absorpt_t_min   0.279
_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:
 C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C13(H13A,H13B,H13C), C12(H12A,H12B,
 H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C14(H14A,
 H14B,H14C), C17(H17A,H17B,H17C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              96131
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.354
_oxdiff_exptl_absorpt_empirical_full_min 0.640