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_1568634
_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         'C16 H27 Br2 Fe P5'
_chemical_formula_sum            'C16 H27 Br2 Fe P5'
_chemical_formula_weight         589.89
_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             2021-12-03
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-12-23 deposited with the CCDC.	2023-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.4910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.35480(10)
_cell_length_b                   14.71550(10)
_cell_length_c                   11.90660(10)
_cell_measurement_reflns_used    20548
_cell_measurement_temperature    123.2(3)
_cell_measurement_theta_max      75.8290
_cell_measurement_theta_min      4.0880
_cell_volume                     2254.91(3)
_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      123.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -71.00 -18.00   1.00    1.50    --  -43.48 122.00  73.00   53
  2  \w   -113.00 -88.00   1.00    1.50    --  -43.48-150.00-169.00   25
  3  \w     51.00  76.00   1.00    1.50    --   43.48-150.00-169.00   25
  4  \w     50.00  95.00   1.00    1.50    --   43.48-122.00  -7.00   45
  5  \w     79.00 109.00   1.00    6.00    --  108.00-122.00  -7.00   30
  6  \w    100.00 125.00   1.00    6.00    --  108.00 150.00-124.00   25
  7  \w    138.00 163.00   1.00    6.00    --  108.00 122.00  73.00   25
  8  \w     95.00 122.00   1.00    6.00    --  108.00-150.00-169.00   27
  9  \w    -68.00  27.00   1.00    1.50    --  -43.48  37.00 -30.00   95
 10  \w   -112.00 -20.00   1.00    1.50    --  -43.48 -37.00 150.00   92
 11  \w    132.00 168.00   1.00    6.00    --  108.00  77.00 -60.00   36
 12  \w     50.00  90.00   1.00    6.00    --  108.00-125.00 -90.00   40
 13  \w     29.00  63.00   1.00    6.00    --  108.00 -94.00 150.00   34
 14  \w     63.00 112.00   1.00    6.00    --  108.00-125.00  30.00   49
 15  \w     88.00 116.00   1.00    6.00    --  108.00  61.00  90.00   28
 16  \w     67.00 100.00   1.00    6.00    --  108.00 -45.00-180.00   33
 17  \w     35.00  82.00   1.00    6.00    --  108.00-125.00  90.00   47
 18  \w     87.00 112.00   1.00    6.00    --  108.00-125.00  90.00   25
 19  \w     97.00 170.00   1.00    6.00    --  108.00 125.00 -90.00   73
 20  \w     53.00 112.00   1.00    6.00    --  108.00-125.00 120.00   59
 21  \w     82.00 108.00   1.00    6.00    --  108.00-125.00  60.00   26
 22  \w    114.00 161.00   1.00    6.00    --  108.00  61.00  60.00   47
 23  \w    108.00 134.00   1.00    6.00    --  108.00 -61.00  30.00   26
 24  \w     98.00 178.00   1.00    6.00    --  108.00 125.00-180.00   80
 25  \w     36.00 134.00   1.00    6.00    --  108.00 -30.00 150.00   98
 26  \w    139.00 165.00   1.00    6.00    --  108.00  61.00  90.00   26
 27  \w     41.00  66.00   1.00    6.00    --  108.00 -77.00  30.00   25
 28  \w    104.00 130.00   1.00    6.00    --  108.00 -77.00  30.00   26
 29  \w    100.00 125.00   1.00    6.00    --  108.00 125.00 150.00   25
 30  \w     43.00  69.00   1.00    6.00    --  108.00 -94.00 -60.00   26
 31  \w     72.00 106.00   1.00    6.00    --  108.00 -94.00 -60.00   34
 32  \w    106.00 178.00   1.00    6.00    --  108.00  77.00  90.00   72
 33  \w     77.00 104.00   1.00    6.00    --  108.00-125.00 -60.00   27
 34  \w     71.00  96.00   1.00    6.00    --  108.00-125.00 -30.00   25
 35  \w     46.00  91.00   1.00    6.00    --  108.00 -94.00-120.00   45
 36  \w     81.00 106.00   1.00    6.00    --  108.00 -94.00   0.00   25
 37  \w     66.00  92.00   1.00    6.00    --  108.00 -94.00  60.00   26
 38  \w     85.00 110.00   1.00    6.00    --  108.00 -45.00-150.00   25
 39  \w     41.00  66.00   1.00    6.00    --  108.00 -61.00 150.00   25
 40  \w    119.00 153.00   1.00    6.00    --  108.00  77.00 -30.00   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0588121000
_diffrn_orient_matrix_UB_12      -0.0787544000
_diffrn_orient_matrix_UB_13      -0.0056286000
_diffrn_orient_matrix_UB_21      0.0907729000
_diffrn_orient_matrix_UB_22      -0.0514574000
_diffrn_orient_matrix_UB_23      0.0298506000
_diffrn_orient_matrix_UB_31      0.0040934000
_diffrn_orient_matrix_UB_32      0.0092916000
_diffrn_orient_matrix_UB_33      0.1175387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32647
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         75.867
_diffrn_reflns_theta_min         4.121
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.596
_exptl_absorpt_correction_T_max  0.578
_exptl_absorpt_correction_T_min  0.029
_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    1.738
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.320
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         6367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0941P)^2^+0.8077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6143
_reflns_number_total             6367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00580a2.cif
_cod_data_source_block           abs_det_gaus
_cod_depositor_comments
'Adding full bibliography for 1568634--1568643.cif.'
_cod_database_code               1568634
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H27Br2FeP5
_shelx_estimated_absorpt_t_max   0.227
_shelx_estimated_absorpt_t_min   0.058
_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:
 C14(H14A,H14B), C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B), C12(H12A,
 H12B), C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C),
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              35358
_shelx_hkl_checksum              32209
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.742
_oxdiff_exptl_absorpt_empirical_full_min 0.651