A 2,2′-diphosphinotolane as a versatile precursor for the synthesis of P-ylidic mesoionic carbenes via reversible C‒P bond formation
Wagner, Hannah K.; Wadepohl, Hubert; Ballmann, Joachim; Chemical Science 12 (2021) 3693–3701; doi:10.1039/D0SC06128J

data_1560224
_publ_section_title
;
 A 2,2&#x2032;-diphosphinotolane as a versatile precursor for the
 synthesis of P-ylidic mesoionic carbenes via reversible C--P bond
 formation
;
_journal_issue                   10
_journal_name_full               'Chemical Science'
_journal_page_first              3693
_journal_page_last               3701
_journal_paper_doi               10.1039/D0SC06128J
_journal_volume                  12
_journal_year                    2021
_chemical_formula_sum            'C45 H60 Cl N O2 P2 Pt'
_chemical_formula_weight         939.42
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_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     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_hw13
_audit_creation_date             2019-04-08
_audit_creation_method
;
encif (version 1.112)

encifer (version_id = 270009.64)

Olex2 1.3
(compiled 2020.01.31 svn.r88ba2a3 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2021-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.9474(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.17660(19)
_cell_length_b                   11.59885(8)
_cell_length_c                   21.4296(2)
_cell_measurement_reflns_used    57822
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      33.9190
_cell_measurement_theta_min      2.4710
_cell_volume                     4096.41(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_publication_material
'encif (Wadepohl, 2009-19); encifer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SIR2019 (Giacovazzo et al., 2019)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.976
_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      2.00 103.00   1.00   20.00    --   32.43  77.00  30.00  101
  2  \w      2.00 103.00   1.00   20.00    --   32.43  77.00-150.00  101
  3  \w    -40.00  58.00   1.00   20.00    --   32.43 -38.00  60.00   98
  4  \w      2.00 103.00   1.00   20.00    --   32.43  77.00 120.00  101
  5  \w    -38.00  62.00   1.00   20.00    --   32.43 -77.00  30.00  100
  6  \w      7.00 105.00   1.00   20.00    --   32.43  38.00   0.00   98
  7  \w    -20.00  74.00   1.00   20.00    --   32.43 -99.00-150.00   94
  8  \w    -40.00  58.00   1.00   20.00    --   32.43 -38.00-120.00   98
  9  \w    -20.00  74.00   1.00   20.00    --   32.43 -99.00 -30.00   94
 10  \w      2.00 103.00   1.00   20.00    --   32.43  77.00 150.00  101
 11  \w      2.00 103.00   1.00   20.00    --   32.43  77.00 -60.00  101
 12  \w    -51.00  47.00   1.00   20.00    --  -25.00  37.00  69.00   98
 13  \w     -5.00  24.00   1.00   20.00    --   28.00  82.00  -5.47   29
 14  \w    -36.00  54.00   1.00   20.00    --   32.43 -57.00 -60.00   90
 15  \w    -40.00  58.00   1.00   20.00    --   32.43 -38.00-180.00   98
 16  \w     12.00 101.00   1.00   20.00    --   32.43  57.00-120.00   89
 17  \w      7.00 105.00   1.00   20.00    --   32.43  38.00 150.00   98
 18  \w      2.00 103.00   1.00   20.00    --   32.43  77.00-120.00  101
 19  \f      0.00  25.00   1.00   20.00 -15.79  32.43 -40.00    --    25
 20  \w    -20.00  74.00   1.00   20.00    --   32.43 -99.00 120.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Agilent SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0429617000
_diffrn_orient_matrix_UB_12      -0.0004402000
_diffrn_orient_matrix_UB_13      0.0173990000
_diffrn_orient_matrix_UB_21      -0.0001268000
_diffrn_orient_matrix_UB_22      -0.0609691000
_diffrn_orient_matrix_UB_23      -0.0025401000
_diffrn_orient_matrix_UB_31      0.0026390000
_diffrn_orient_matrix_UB_32      0.0045870000
_diffrn_orient_matrix_UB_33      -0.0320000000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            210353
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.806
_diffrn_reflns_theta_min         2.147
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.607
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.629
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
 a multifaceted crystal model (Busing & Levy, 1957).
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.051
_refine_diff_density_max         2.467
_refine_diff_density_min         -2.656
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         17347
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0176P)^2^+6.1104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14940
_reflns_number_total             17347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06128j2.cif
_cod_data_source_block           ba_hw13_sq
_cod_depositor_comments
'Adding full bibliography for 1560218--1560233.cif.'
_cod_original_cell_volume        4096.41(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1560224
_audit_block_refno               3319
_audit_block_usercomment         'HW148, block, yellow'
_shelx_estimated_absorpt_t_max   0.714
_shelx_estimated_absorpt_t_min   0.714
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     33.07
_shelxl_version_number           2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O51, C52, C53, C54, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C15(H15), C18(H18), C21(H21), C24(H24)
3.b Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C14(H14),
 C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_hkl_checksum              4686
_shelx_fab_checksum              58536
_platon_squeeze_void_probe_radius 1.20
_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 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.906
_shelx_res_checksum              31212
_cell_oxdiff_length_a            18.1774(3)
_cell_oxdiff_length_b            11.60075(17)
_cell_oxdiff_length_c            21.4288(3)
_cell_oxdiff_angle_alpha         90.0036(12)
_cell_oxdiff_angle_beta          114.9681(16)
_cell_oxdiff_angle_gamma         90.0171(13)
_cell_oxdiff_volume              4096.41(10)
_cell_oxdiff_measurement_reflns_used 57599