Substituted aromatic pentaphosphole ligands ‒ a journey across the p-block
Riesinger, Christoph; Balázs, Gábor; Seidl, Michael; Scheer, Manfred; Chemical Science  (2021) –; doi:10.1039/D1SC04296C

data_1564642
_publ_section_title
;
 Substituted aromatic pentaphosphole ligands -- a journey across the
 p-block
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04296C
_journal_year                    2021
_chemical_formula_moiety         'C22 H26 Fe P5 Si, B C24 F20'
_chemical_formula_sum            'C46 H26 B F20 Fe P5 Si'
_chemical_formula_weight         1208.27
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-02
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-05-13 deposited with the CCDC.	2021-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.070(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0141(2)
_cell_length_b                   14.79290(10)
_cell_length_c                   20.3007(3)
_cell_measurement_reflns_used    19875
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      72.9960
_cell_measurement_theta_min      2.8190
_cell_volume                     4700.82(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.15
_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 0.965
_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     49.00 121.00   0.50    1.00    --   75.28  15.00  60.00  144
  2  \w     65.00 110.00   0.50    1.00    --   62.52  25.00 -10.00   90
  3  \w     73.00 108.00   0.50    1.00    --   75.28  25.00 -10.00   70
  4  \w     39.00 113.00   0.50    1.00    --   75.56   0.00 -30.00  148
  5  \w     25.00  98.00   0.50    1.00    --   62.52   0.00 -90.00  146
  6  \w     34.00  96.00   0.50    1.00    --   62.52   0.00-180.00  124
  7  \w     15.00  41.00   0.50    1.00    --   62.52 -25.00-174.00   52
  8  \w     35.00  71.00   0.50    1.00    --   62.52 -95.00-120.00   72
  9  \w     23.00  89.00   0.50    1.00    --   62.52-125.00-150.00  132
 10  \w     58.00  84.00   0.50    1.00    --   75.56 -95.00 -90.00   52
 11  \w     43.00  82.00   0.50    1.00    --   75.56 -95.00 -30.00   78
 12  \w     39.00  84.00   0.50    1.00    --   75.28 -95.00   0.00   90
 13  \w     37.00 104.00   0.50    1.00    --   75.28-125.00  90.00  134
 14  \w     38.00  82.00   0.50    1.00    --   75.56 -95.00  90.00   88
 15  \w    -99.00 -26.00   0.50    1.00    --  -70.22 125.00  60.00  146
 16  \w    -94.00 -68.00   0.50    1.00    --  -70.22 -25.00-174.00   52
 17  \w   -111.00 -86.00   0.50    1.00    --  -63.96 -25.00-174.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33445
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.459
_diffrn_reflns_theta_min         2.823
_exptl_absorpt_coefficient_mu    5.490
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_description       plate
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.649
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         9127
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0359
_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^)+(0.0637P)^2^+1.5238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8217
_reflns_number_total             9127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr752
_cod_original_cell_volume        4700.82(11)
_cod_database_code               1564642
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.771
_shelx_estimated_absorpt_t_min   0.378
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22B-C17 \\sim C22A-C17 \\sim C16-C21B \\sim C21A-C16
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C17 \\sim C22B \\sim C22A \\sim C16 \\sim C21B \\sim C21A: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
4. Others
 Fixed Sof: C21A(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C22B(0.5) H22A(0.5)
 H22B(0.5) H22C(0.5) C21B(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C22A(0.5)
 H22D(0.5) H22E(0.5) H22F(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C5(H5), C3(H3), C4(H4), C8(H8), C12(H12), C9(H9), C11(H11),
 C10(H10)
5.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C21A(H21A,H21B,
 H21C), C22B(H22A,H22B,H22C), C21B(H21D,H21E,H21F), C22A(H22D,H22E,H22F)
;
_shelx_res_checksum              15276
_shelx_hkl_checksum              23787
_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
;