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_1568637
_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         'C13 H21 Fe P5'
_chemical_formula_sum            'C13 H21 Fe P5'
_chemical_formula_weight         388.00
_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
_audit_creation_date             2021-07-07
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_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                   8.47550(10)
_cell_length_b                   8.84210(10)
_cell_length_c                   22.8473(3)
_cell_measurement_reflns_used    6791
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.0080
_cell_measurement_theta_min      3.8680
_cell_volume                     1712.20(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      123.00(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 0.999
_diffrn_measured_fraction_theta_max 0.986
_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     31.00  58.00   0.50    0.10    --   62.57  15.00 150.00   54
  2  \w     63.00  98.00   0.50    0.10    --   62.57  15.00 150.00   70
  3  \w     46.00 120.00   0.50    0.22    --   75.21  15.00  60.00  148
  4  \w     51.00 107.00   0.50    0.22    --   75.21  15.00-180.00  112
  5  \w    -67.00 -37.00   0.50    0.10    --  -64.16 -15.00-180.00   60
  6  \w   -108.00 -83.00   0.50    0.10    --  -64.16 -15.00-180.00   50
  7  \w     53.00  80.00   0.50    0.22    --   75.63 -95.00-120.00   54
  8  \w     60.00  85.00   0.50    0.22    --   75.63-110.00  71.00   50
  9  \w     40.00  65.00   0.50    0.22    --   75.21-110.00  71.00   50
 10  \w     51.00  76.00   0.50    0.10    --   62.57-110.00  71.00   50
 11  \w     38.00  99.00   0.50    0.22    --   75.21-125.00 120.00  122
 12  \w     39.00  78.00   0.50    0.22    --   75.63 -95.00 120.00   78
 13  \w    -86.00 -42.00   0.50    0.10    --  -70.24 110.00 165.00   88
 14  \w    -55.00 -29.00   0.50    0.10    --  -64.16 110.00 165.00   52
 15  \w    -99.00 -66.00   0.50    0.10    --  -70.24 125.00-120.00   66
 16  \w    -56.00 -30.00   0.50    0.10    --  -70.24 125.00-120.00   52
;
_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      0.1608735000
_diffrn_orient_matrix_UB_12      -0.0042576000
_diffrn_orient_matrix_UB_13      -0.0313853000
_diffrn_orient_matrix_UB_21      0.0807299000
_diffrn_orient_matrix_UB_22      -0.0442975000
_diffrn_orient_matrix_UB_23      0.0579247000
_diffrn_orient_matrix_UB_31      -0.0250500000
_diffrn_orient_matrix_UB_32      -0.1684253000
_diffrn_orient_matrix_UB_33      -0.0144740000
_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  0.0258
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8327
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.928
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.258
_diffrn_reflns_theta_min         3.870
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.350
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.122
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1194 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0511P)^2^+0.4777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.625
_reflns_Friedel_fraction_full    0.920
_reflns_Friedel_fraction_max     0.848
_reflns_number_gt                3167
_reflns_number_total             3197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00580a2.cif
_cod_data_source_block           abs_gaus_error5_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1568634--1568643.cif.'
_cod_database_code               1568637
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C13H21FeP5
_shelx_estimated_absorpt_t_max   0.464
_shelx_estimated_absorpt_t_min   0.127
_reflns_odcompleteness_completeness 99.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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:
 C11(H11A,H11B), C13(H13A,H13B), C12(H12A,H12B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,H10B,H10C),
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              43028
_shelx_hkl_checksum              3936
_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 1.929
_oxdiff_exptl_absorpt_empirical_full_min 0.582