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_1568635
_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_absolute_configuration ad
_chemical_formula_moiety         'C15 H25 Fe P5'
_chemical_formula_sum            'C15 H25 Fe P5'
_chemical_formula_weight         416.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.12.02 svn.rb8f36f48 for OlexSys, GUI svn.r6436)
;
_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            4
_cell_length_a                   9.17120(10)
_cell_length_b                   14.22010(10)
_cell_length_c                   14.9030(2)
_cell_measurement_reflns_used    13178
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.0200
_cell_measurement_theta_min      4.2630
_cell_volume                     1943.58(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-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      123.01(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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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     29.00  57.00   0.50    0.05    --   62.55-145.00 -91.00   56
  2  \w     26.00  56.00   0.50    0.05    --   62.55-126.00  75.00   60
  3  \w    -89.00 -64.00   0.50    0.05    --  -64.35 145.00 -39.00   50
  4  \w    -71.00 -45.00   0.50    0.05    --  -68.39 126.00 152.00   52
  5  \w    -79.00 -54.00   0.50    0.05    --  -68.39 145.00 -39.00   50
  6  \w     49.00  74.00   0.50    0.05    --   73.48-145.00 -91.00   50
  7  \w     51.00  76.00   0.50    0.05    --   75.18-145.00 -91.00   50
  8  \w     43.00  68.00   0.50    0.05    --   75.18-126.00  75.00   50
  9  \w     71.00  97.00   0.50    0.05    --   75.18 145.00 -39.00   52
 10  \w     72.00 100.00   0.50    0.05    --   62.55  15.00 150.00   56
 11  \w     37.00  69.00   0.50    0.05    --   62.55  15.00 150.00   64
 12  \w    -69.00 -39.00   0.50    0.05    --  -64.35 -15.00  90.00   60
 13  \w    -52.00 -25.00   0.50    0.05    --  -64.35 125.00  30.00   54
 14  \w    -87.00 -29.00   0.50    0.05    --  -64.35 125.00-150.00  116
 15  \w    -86.00 -57.00   0.50    0.05    --  -64.35 125.00  30.00   58
 16  \w     50.00  96.00   0.50    0.05    --   75.18-125.00  90.00   92
 17  \w     36.00  98.00   0.50    0.05    --   75.18-125.00 150.00  124
 18  \w     43.00  93.00   0.50    0.05    --   75.18-125.00  60.00  100
 19  \w     49.00  78.00   0.50    0.05    --   77.75 -92.00  83.70   58
 20  \w     48.00  73.00   0.50    0.05    --   77.75 -84.00  27.26   50
 21  \w     68.00  94.00   0.50    0.05    --   77.75  14.00 -80.63   52
 22  \w     39.00  88.00   0.50    0.05    --   77.75-124.00 -13.91   98
 23  \w     60.00 119.00   0.50    0.05    --   77.75  19.00  82.49  118
 24  \w     52.00 113.00   0.50    0.05    --   77.75  18.00  28.67  122
 25  \w     69.00 113.00   0.50    0.05    --   77.75   8.00 152.62   88
 26  \w     65.00  90.00   0.50    0.05    --   77.75  21.00-104.47   50
 27  \w     52.00  82.00   0.50    0.05    --   77.75-120.00 -95.09   60
 28  \w     65.00 110.00   0.50    0.05    --   77.75  21.00 138.92   90
 29  \w     73.00 114.00   0.50    0.05    --   77.75-152.00  -2.96   82
 30  \w     60.00 114.00   0.50    0.05    --   77.75   7.00-134.28  108
 31  \w     58.00  95.00   0.50    0.05    --   77.75   8.00  81.38   74
 32  \w     70.00 100.00   0.50    0.05    --   77.75   3.00 122.67   60
 33  \w     79.00 106.00   0.50    0.05    --   77.75  20.00 -60.53   54
;
_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      0.1412352000
_diffrn_orient_matrix_UB_12      0.0386935000
_diffrn_orient_matrix_UB_13      0.0419999000
_diffrn_orient_matrix_UB_21      0.0579142000
_diffrn_orient_matrix_UB_22      0.0245716000
_diffrn_orient_matrix_UB_23      -0.0941777000
_diffrn_orient_matrix_UB_31      -0.0700306000
_diffrn_orient_matrix_UB_32      0.0982088000
_diffrn_orient_matrix_UB_33      0.0069463000
_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  0.0303
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20511
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.432
_diffrn_reflns_theta_min         4.297
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.036
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.254
_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    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 1576 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0153P)^2^+1.6641P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0592
_reflns_Friedel_coverage         0.746
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                3896
_reflns_number_total             3935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00580a2.cif
_cod_data_source_block           abs_gaus_error5
_cod_depositor_comments
'Adding full bibliography for 1568634--1568643.cif.'
_cod_database_code               1568635
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H25FeP5
_shelx_estimated_absorpt_t_max   0.540
_shelx_estimated_absorpt_t_min   0.314
_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:
 C15(H15A,H15B), C11(H11A,H11B), C14(H14A,H14B), C12(H12A,H12B), C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C),
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              86718
_shelx_hkl_checksum              64910
_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 1.278
_oxdiff_exptl_absorpt_empirical_full_min 0.808