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_1568636
_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         'C14 H23 Fe P5'
_chemical_formula_sum            'C14 H23 Fe P5'
_chemical_formula_weight         402.02
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-21
_audit_creation_method
;
Olex2 1.5-alpha
(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                69.087(2)
_cell_angle_beta                 77.735(2)
_cell_angle_gamma                89.910(2)
_cell_formula_units_Z            4
_cell_length_a                   9.4353(2)
_cell_length_b                   13.7981(3)
_cell_length_c                   15.3668(4)
_cell_measurement_reflns_used    16741
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.4500
_cell_measurement_theta_min      3.1430
_cell_volume                     1820.09(8)
_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-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (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      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.947
_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     75.00 115.00   0.50    0.10    --   74.95  15.00  30.00   80
  2  \w     43.00 102.00   0.50    0.05    --   62.44  15.00  90.00  118
  3  \w     68.00 104.00   0.50    0.10    --   74.95  15.00 120.00   72
  4  \w     39.00 102.00   0.50    0.05    --   62.44  15.00-120.00  126
  5  \w     77.00 103.00   0.50    0.05    --   62.44  15.00-180.00   52
  6  \w     36.00  62.00   0.50    0.05    --   62.44  15.00-180.00   52
  7  \w     48.00 113.00   0.50    0.10    --   74.95  15.00-180.00  130
  8  \w     60.00 113.00   0.50    0.10    --   74.95  15.00 -90.00  106
  9  \w     52.00 115.00   0.50    0.10    --   74.95  15.00 -30.00  126
 10  \w     48.00  97.00   0.50    0.10    --   76.87-117.00  53.75   98
 11  \w     26.00  64.00   0.50    0.05    --   62.44-125.00 150.00   76
 12  \w     43.00  86.00   0.50    0.05    --   62.44-125.00  30.00   86
 13  \w     35.00  61.00   0.50    0.05    --   72.51-125.00  30.00   52
 14  \w     36.00  61.00   0.50    0.05    --   72.51-125.00  90.00   50
 15  \w     49.00  99.00   0.50    0.10    --   74.95-125.00 150.00  100
 16  \w     67.00  93.00   0.50    0.05    --   72.51-125.00  90.00   52
 17  \w     67.00  93.00   0.50    0.05    --   72.51-125.00  30.00   52
 18  \w     37.00  99.00   0.50    0.10    --   74.95-125.00   0.00  124
 19  \w     74.00  99.00   0.50    0.10    --   74.95-125.00 -60.00   50
 20  \w     74.00  99.00   0.50    0.10    --   74.95-125.00 -90.00   50
 21  \w     43.00  82.00   0.50    0.05    --   62.44-125.00-180.00   78
 22  \w     52.00 109.00   0.50    0.10    --   76.87-139.00-146.94  114
 23  \w     29.00  83.00   0.50    0.05    --   62.44-125.00 -60.00  108
 24  \w     74.00  99.00   0.50    0.10    --   74.95-125.00-120.00   50
 25  \w     53.00  97.00   0.50    0.10    --   76.87-118.00 -40.35   88
 26  \w     74.00  99.00   0.50    0.10    --   74.95-125.00  30.00   50
 27  \w     46.00  97.00   0.50    0.10    --   76.87-118.00 102.05  102
 28  \w   -106.00 -43.00   0.50    0.10    --  -74.00 144.00 151.55  126
 29  \w    -92.00 -31.00   0.50    0.05    --  -68.24 125.00 150.00  122
 30  \w    -63.00 -37.00   0.50    0.05    --  -64.34 125.00 120.00   52
 31  \w    -89.00 -46.00   0.50    0.05    --  -68.24 125.00   0.00   86
 32  \w    -88.00 -37.00   0.50    0.10    --  -74.00 110.00-101.87  102
 33  \w    -69.00 -44.00   0.50    0.05    --  -64.34 -15.00-150.00   50
 34  \w   -104.00 -77.00   0.50    0.05    --  -64.34 -15.00-150.00   54
 35  \w   -106.00 -42.00   0.50    0.05    --  -68.24 -15.00 -90.00  128
 36  \w   -100.00 -60.00   0.50    0.05    --  -68.24 -15.00   0.00   80
;
_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      0.1530480000
_diffrn_orient_matrix_UB_12      -0.0398744000
_diffrn_orient_matrix_UB_13      -0.0067992000
_diffrn_orient_matrix_UB_21      0.0219380000
_diffrn_orient_matrix_UB_22      0.0373211000
_diffrn_orient_matrix_UB_23      0.0798574000
_diffrn_orient_matrix_UB_31      -0.0648098000
_diffrn_orient_matrix_UB_32      -0.1067623000
_diffrn_orient_matrix_UB_33      0.0756259000
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23461
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.907
_diffrn_reflns_theta_min         3.161
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.697
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.231
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6987
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0641P)^2^+1.2136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6827
_reflns_number_total             6987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00580a2.cif
_cod_data_source_block           abs_gaus_erroro5
_cod_depositor_comments
'Adding full bibliography for 1568634--1568643.cif.'
_cod_database_code               1568636
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H15FeP5C4H8
_shelx_estimated_absorpt_t_max   0.224
_shelx_estimated_absorpt_t_min   0.043
_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.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C14(H14A,H14B), C11(H11A,H11B), C13(H13A,H13B), C12(H12A,
 H12B), C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C24(H24A,H24B,H24C),
 C20(H20A,H20B,H20C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              2415
_shelx_hkl_checksum              1281
_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 1.983
_oxdiff_exptl_absorpt_empirical_full_min 0.730