Novel synthetic route for (parent) phosphetanes, phospholanes, phosphinanes and phosphepanes.
Reichl, Stephan; Balázs, Gábor; Scheer, Manfred; Chemical science 14 (2023) 3834–3838; doi:10.1039/d3sc00580a

data_1568643
_publ_section_title
;
 Novel synthetic route for (parent) phosphetanes, phospholanes,
 phosphinanes and phosphepanes.
;
_journal_issue                   14
_journal_name_full               'Chemical science'
_journal_page_first              3834
_journal_page_last               3838
_journal_paper_doi               10.1039/d3sc00580a
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C8 H18 Cl2 P2 Pt'
_chemical_formula_sum            'C8 H18 Cl2 P2 Pt'
_chemical_formula_weight         442.15
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-02-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-12-23 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.67740(10)
_cell_length_b                   11.67740(10)
_cell_length_c                   18.9131(2)
_cell_measurement_reflns_used    119891
_cell_measurement_temperature    100.01(12)
_cell_measurement_theta_max      44.2860
_cell_measurement_theta_min      2.4630
_cell_volume                     2579.02(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(12)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_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     30.00  64.00   0.50   10.00    --   17.83  42.00 175.84   68
  2  \w     21.00  53.00   0.50   10.00    --   17.83  78.00 -43.26   64
  3  \w     16.00  45.00   0.50   10.00    --   17.83  86.00-121.62   58
  4  \w     16.00  45.00   0.50   10.00    --   17.83  85.00  95.58   58
  5  \w    -29.00  34.00   0.50   10.00    --   17.83 -22.00 178.01  126
  6  \w    -29.00  26.00   0.50   10.00    --   17.83 -25.00 124.81  110
  7  \w    -28.00  32.00   0.50   10.00    --   17.83 -19.00  60.00  120
  8  \w    -29.00  15.00   0.50   10.00    --   17.83 -29.00 168.22   88
  9  \w    -29.00  32.00   0.50   10.00    --   17.83 -23.00 -68.64  122
 10  \w     10.00  36.00   0.50   10.00    --   17.83  94.00 -71.53   52
 11  \w     17.00  45.00   0.50   10.00    --   17.83  84.00-168.11   56
 12  \w    -29.00  26.00   0.50   10.00    --   17.83 -25.00-123.53  110
 13  \w     10.00  36.00   0.50   10.00    --   17.83  94.00 133.59   52
 14  \w     31.00  64.00   0.50   10.00    --   17.83  41.00  37.83   66
 15  \w     10.00  36.00   0.50   10.00    --   17.83  94.00  16.32   52
 16  \w     31.00  64.00   0.50   10.00    --   17.83  40.00 -27.09   66
 17  \w     28.00  61.00   0.50   10.00    --   17.83  56.00-160.00   66
 18  \w    -28.00  32.00   0.50   10.00    --   18.00 -20.00  11.28  120
 19  \w     27.00  59.00   0.50   10.00    --   18.00  62.00  47.83   64
 20  \w     27.00  59.00   0.50   10.00    --   18.00  62.00 -67.04   64
 21  \w    -14.00  62.00   0.50   10.00    --   18.00  12.00 138.77  152
 22  \w     10.00  65.00   0.50   10.00    --   18.00  25.00  24.71  110
 23  \w     -4.00  64.00   0.50   10.00    --   18.00  20.00 -86.09  136
 24  \w     23.00  66.00   0.50   10.00    --   18.00  30.00 155.66   86
 25  \w     14.00  45.00   0.50   10.00    --   18.00  88.00  52.32   62
 26  \w     17.00  66.00   0.50   10.00    --   18.00  27.00 -62.31   98
 27  \w    -29.00  12.00   0.50   10.00    --   18.00 -32.00 -57.55   82
 28  \w     27.00  59.00   0.50   10.00    --   18.00  62.00   0.84   64
 29  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00  28.28   78
 30  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 126.80   78
 31  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00  82.48   78
 32  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 -90.94   78
 33  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 -43.20   78
 34  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00-144.66   78
 35  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00-109.05   78
 36  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 -58.61   78
 37  \w    -43.00  -5.00   0.50   10.00    --  -18.45 117.00 104.43   76
 38  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 -10.13   78
 39  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00  59.45   78
 40  \w    -19.00  16.00   0.50   10.00    --  -18.45  83.00 -73.10   70
 41  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 170.59   78
 42  \w    -27.00   6.00   0.50   10.00    --   17.83 -49.00 -69.13   66
 43  \w     -9.00  64.00   0.50   10.00    --   17.83  19.00 -30.00  146
 44  \w     29.00  61.00   0.50   10.00    --   17.83  55.00-122.25   64
 45  \w    -29.00  19.00   0.50   10.00    --   17.83 -27.00-124.14   96
 46  \w    -28.00  32.00   0.50   10.00    --   17.83 -19.00 -60.00  120
 47  \w    -19.00  28.00   0.50   10.00    --   17.83   0.00   0.00   94
 48  \w    -28.00  33.00   0.50   10.00    --   17.83 -21.00 -26.36  122
 49  \w    -19.00  55.00   0.50   10.00    --   17.83   0.00 -90.00  148
 50  \w    -28.00  32.00   0.50   10.00    --   17.83 -19.00  90.00  120
 51  \w    -29.00  26.00   0.50   10.00    --   17.83 -25.00 -25.86  110
 52  \w    -29.00   9.00   0.50   10.00    --   17.83 -35.00-124.81   76
 53  \w     29.00  62.00   0.50   10.00    --   17.83  51.00 175.33   66
 54  \w    -29.00  22.00   0.50   10.00    --   17.83 -26.00 173.00  102
 55  \w     -9.00  64.00   0.50   10.00    --   17.83  19.00-180.00  146
 56  \w    -23.00   9.00   0.50   10.00    --   17.83 -62.00  40.76   64
 57  \w     28.00  60.00   0.50   10.00    --   18.00  59.00  91.15   64
 58  \w    -28.00  28.00   0.50   10.00    --  -18.45  19.00 -30.00  112
 59  \w    -30.00  29.00   0.50   10.00    --  -18.45  24.00   2.22  118
 60  \w    -22.00  17.00   0.50   10.00    --  -18.45  88.00   8.08   78
 61  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 -81.74   78
 62  \w    -43.00  -5.00   0.50   10.00    --  -18.45 117.00 -70.89   76
 63  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 155.15   78
 64  \w    -42.00  -4.00   0.50   10.00    --  -18.45 115.00 -26.26   76
 65  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00  71.68   78
 66  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00 -18.00   78
 67  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00  10.00   78
 68  \w    -44.00  -7.00   0.50   10.00    --  -18.45 119.00-123.74   74
 69  \w    -56.00 -19.00   0.50   10.00    --  -18.45 141.00  32.49   74
 70  \w    -17.00  16.00   0.50   10.00    --  -18.45  80.00  24.79   66
 71  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00  95.94   78
 72  \w    -45.00  -8.00   0.50   10.00    --  -18.45 121.00-112.99   74
 73  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00-134.53   78
 74  \w    -42.00  -4.00   0.50   10.00    --  -18.45 115.00  15.96   76
 75  \w    -43.00  -4.00   0.50   10.00    --  -18.45 116.00-168.59   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0182537000
_diffrn_orient_matrix_UB_12      -0.0382777000
_diffrn_orient_matrix_UB_13      0.0268391000
_diffrn_orient_matrix_UB_21      0.0518804000
_diffrn_orient_matrix_UB_22      0.0311300000
_diffrn_orient_matrix_UB_23      0.0034824000
_diffrn_orient_matrix_UB_31      -0.0258204000
_diffrn_orient_matrix_UB_32      0.0353764000
_diffrn_orient_matrix_UB_33      0.0259750000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            192001
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.546
_diffrn_reflns_theta_min         2.467
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    11.502
_exptl_absorpt_correction_T_max  0.731
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.83a (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.076
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.857
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Flack x determined using 1029 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+8.0897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0495
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2300
_reflns_number_total             2350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00580a2.cif
_cod_data_source_block           abs_066_gaus
_cod_depositor_comments
'Adding full bibliography for 1568634--1568643.cif.'
_cod_original_cell_volume        2579.02(5)
_cod_database_code               1568643
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C8H18Cl2P2Pt
_shelx_estimated_absorpt_t_max   0.656
_shelx_estimated_absorpt_t_min   0.475
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: Pt01(0.26) Pt(0.24)
3.a Secondary CH2 refined with riding coordinates:
 C005(H00A,H00B), C006(H00C,H00D), C1(H1A,H1B), C2(H2A,H2B)
;
_shelx_res_checksum              90626
_shelx_hkl_checksum              73722
_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 2.999
_oxdiff_exptl_absorpt_empirical_full_min 0.410