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_7715984
_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 P3 Ru'
_chemical_formula_sum            'C20 H33 P3 Ru'
_chemical_formula_weight         467.44
_chemical_name_systematic        '[Cp*Ru(?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                 107.637(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2485(5)
_cell_length_b                   13.0851(5)
_cell_length_c                   16.3300(9)
_cell_measurement_reflns_used    13391
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      67.2810
_cell_measurement_theta_min      4.3940
_cell_volume                     2086.96(18)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 41.104a 64-bit (release 16-03-2021))'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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     16.00 113.00   1.00   22.00    --   89.50 -29.00  90.00   97
  2  \w     12.00  86.00   1.00   22.00    --   89.50-103.00 -15.00   74
  3  \w   -166.00-101.00   1.00   22.00    --  -90.00-107.00-108.00   65
  4  \w     32.00  86.00   1.00    6.00    --    0.00-178.00   0.00   54
  5  \w     35.00  88.00   1.00    6.00    --    0.00 178.00 -90.00   53
  6  \w    -18.00  43.00   1.00    6.00    --    0.00-107.00-108.00   61
  7  \w   -120.00 -18.00   1.00   22.00    --  -90.00  77.00  90.00  102
  8  \w   -162.00 -94.00   1.00   22.00    --  -90.00-125.00   0.00   68
  9  \w   -171.00-101.00   1.00   22.00    --  -90.00 -95.00 120.00   70
 10  \w   -113.00 -21.00   1.00   22.00    --  -90.00  45.00  30.00   92
 11  \w   -115.00 -21.00   1.00   22.00    --  -90.00  61.00-120.00   94
 12  \w    -72.00  30.00   1.00    6.00    --    0.00 -77.00  60.00  102
 13  \w    -69.00  24.00   1.00    6.00    --    0.00 -57.00 150.00   93
 14  \w     67.00 158.00   1.00   22.00    --   89.50  45.00-120.00   91
 15  \w     67.00 158.00   1.00   22.00    --   89.50  45.00  30.00   91
 16  \w     64.00 112.00   1.00   22.00    --   89.50  61.00 -60.00   48
 17  \w     67.00 158.00   1.00   22.00    --   89.50  45.00 150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, TitanS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0923752000
_diffrn_orient_matrix_UB_12      0.0929839000
_diffrn_orient_matrix_UB_13      -0.0352303000
_diffrn_orient_matrix_UB_21      0.1279194000
_diffrn_orient_matrix_UB_22      0.0649650000
_diffrn_orient_matrix_UB_23      0.0052108000
_diffrn_orient_matrix_UB_31      -0.0090138000
_diffrn_orient_matrix_UB_32      -0.0319159000
_diffrn_orient_matrix_UB_33      -0.0921262000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17208
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.067
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_min         4.415
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.234
_exptl_absorpt_correction_T_max  0.479
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00085(7)
_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   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.6989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3599
_reflns_number_total             3671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01067a2.cif
_cod_data_source_block           mu117_mp
_cod_depositor_comments
'Adding full bibliography for 7715982--7715988.cif.'
_cod_database_code               7715984
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H33 P3 Ru'
_shelx_estimated_absorpt_t_max   0.438
_shelx_estimated_absorpt_t_min   0.253
_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:
 C16(H16A,H16B,H16C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C12(H12A,
 H12B,H12C), C20(H20A,H20B,H20C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              8298
_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 1.565
_oxdiff_exptl_absorpt_empirical_full_min 0.754