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_1564641
_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         'C20 H30 Fe2 Ga I2 P10, Al C16 F36 O4'
_chemical_formula_sum            'C36 H30 Al F36 Fe2 Ga I2 O4 P10'
_chemical_formula_weight         1982.50
_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             2021-03-05
_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                112.4860(10)
_cell_angle_beta                 95.1250(10)
_cell_angle_gamma                110.9810(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8777(2)
_cell_length_b                   16.0557(2)
_cell_length_c                   18.4470(3)
_cell_measurement_reflns_used    25090
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.4390
_cell_measurement_theta_min      4.0540
_cell_volume                     3175.29(9)
_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(1)
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.973
_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    -66.00  36.00   0.50    6.00    --  -40.03  57.00 -30.00  204
  2  \w    -98.00 -18.00   0.50    6.00    --  -40.03 125.00 -30.00  160
  3  \w      5.00 122.00   0.50    6.00    --   40.03  77.00-180.00  234
  4  \w    -37.00  43.00   0.50    6.00    --   40.03 -38.00  60.00  160
  5  \w     18.00 145.00   0.50   24.00    --  105.16 -90.00   7.74  254
  6  \w     73.00 178.00   0.50   24.00    --  105.16  61.00 -60.00  210
  7  \w     76.00 178.00   0.50   24.00    --  105.16  45.00 150.00  204
  8  \w     70.00 178.00   0.50   24.00    --  105.16  77.00-180.00  216
  9  \w     29.00  71.00   0.50   24.00    --  105.16 -61.00-120.00   84
 10  \w     70.00 178.00   0.50   24.00    --  105.16  77.00  90.00  216
 11  \w     19.00 145.00   0.50   24.00    --  105.16 -91.00 133.08  252
 12  \w     73.00 178.00   0.50   24.00    --  105.16  61.00  30.00  210
 13  \w     19.00 145.00   0.50   24.00    --  105.16 -91.00-120.67  252
 14  \w     35.00 134.00   0.50   24.00    --  105.16 178.00-180.00  198
 15  \w   -122.00  -5.00   0.50    6.00    --  -40.03 -77.00  60.00  234
 16  \w    -98.00 -18.00   0.50    6.00    --  -40.03 125.00 150.00  160
 17  \w      5.00 122.00   0.50    6.00    --   40.03  77.00   0.00  234
 18  \w      9.00 116.00   0.50    6.00    --   40.03  57.00 120.00  214
 19  \w      9.00 116.00   0.50    6.00    --   40.03  57.00 -60.00  214
 20  \w     70.00 178.00   0.50   24.00    --  105.16  77.00 -30.00  216
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33614
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.666
_diffrn_reflns_theta_min         3.830
_exptl_absorpt_coefficient_mu    15.621
_exptl_absorpt_correction_T_max  0.308
_exptl_absorpt_correction_T_min  0.032
_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            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.074
_exptl_crystal_description       plate
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.417
_exptl_crystal_size_mid          0.374
_exptl_crystal_size_min          0.117
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         12088
_refine_ls_number_restraints     851
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0477
_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^)+(0.0853P)^2^+5.6636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1314
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11702
_reflns_number_total             12088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr383_cua
_cod_database_code               1564641
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.262
_shelx_estimated_absorpt_t_min   0.059
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C32B-C29 = C30B-C29
 1.55 with sigma of 0.02
 F30A-C34A \\sim F28-C34A \\sim F29A-C34A \\sim F32A-C35A \\sim F33A-C35A \\sim
F31A-C35A
 with sigma of 0.02
 F30B-C34B \\sim F35B-C36B \\sim F36B-C36B \\sim F34B-C36B \\sim F32B-C35B
\\sim F33B-C35B \\sim F31B-
 C35B
 with sigma of 0.02
 F35B-F36B \\sim F36B-F34B \\sim F34B-F35B
 with sigma of 0.04
 F32B-F33B \\sim F33B-F31B \\sim F31B-F32B
 with sigma of 0.04
 F28-C34A \\sim F28-C34B \\sim F29A-C34B \\sim F29A-C34A \\sim F30A-C34A \\sim
F30B-C34B
 with sigma of 0.02
 F29B-C34B \\sim F29A-C34A
 with sigma of 0.02
 F36A-C36A \\sim F34A-C36A \\sim F35A-C36A
 with sigma of 0.04
 F36A-F34A \\sim F34A-F35A \\sim F35A-F36A
 with sigma of 0.04
 F19-F20 \\sim F20-F21B \\sim F21B-F19
 with sigma of 0.02
 F27B-C32B \\sim F26B-C32B \\sim F25-C32B
 with sigma of 0.02
 C23B-C21 \\sim C21-C23A \\sim C22B-C21 \\sim C21-C22A \\sim C24B-C21 \\sim
C21-C24A
 with sigma of 0.02
 F7-C24B \\sim F9B-C24B \\sim F8B-C24B
 with sigma of 0.02
 F6B-C23B \\sim F4-C23B \\sim F5-C23B
 with sigma of 0.02
 F3B-C22B \\sim F1-C22B \\sim F2B-C22B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F35B \\sim C35A \\sim F32A \\sim F33A \\sim F31A \\sim F32B \\sim C35B \\sim
F33B \\sim F31B: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.9A
C25 \\sim C27A \\sim C27B \\sim F13B \\sim F13A \\sim F14B \\sim F14A \\sim
F15B \\sim F15A: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.9A
F36B \\sim F34B \\sim C36B \\sim F35B \\sim F34A \\sim C36A \\sim F36A \\sim
F35A: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.9A
C34B \\sim F30B \\sim F30A \\sim C34A \\sim F28 \\sim F29A \\sim F29B: within
1.9A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.9A
C25 \\sim C28A \\sim C28B \\sim F16B \\sim F16A \\sim F17A \\sim F17B \\sim
F18A \\sim F18B: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.9A
C36A \\sim F36A \\sim F34A \\sim F35A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
F19 \\sim F20 \\sim C30B \\sim F21B: within 1.9A with sigma of 0.02 and sigma
for terminal atoms of 0.02 within 1.9A
C31B \\sim C31A: within 1.9A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.9A
F24B \\sim C31B: within 1.9A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.9A
F26B \\sim C32B \\sim F25 \\sim F27B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
C23B \\sim C23A \\sim C21 \\sim C22A \\sim C22B \\sim C24B \\sim C24A: within
1.9A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.9A
F3B \\sim C22B \\sim F2B \\sim F1: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F6B \\sim F5 \\sim C23B \\sim F4: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F9B \\sim C24B \\sim F7 \\sim F8B: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
4. Others
 Fixed Sof: F24A(0.85) F26A(0.85) F27A(0.85) F21A(0.85) F18A(0.42) F13A(0.42)
 F17A(0.42) C31A(0.85) F15A(0.42) F14A(0.42) C32A(0.85) F16A(0.42) C30A(0.85)
 C28A(0.42) C27A(0.42) F18B(0.58) F13B(0.58) F17B(0.58) F15B(0.58) F14B(0.58)
 F16B(0.58) C28B(0.58) C27B(0.58) F24B(0.15) F21B(0.15) F26B(0.15) F27B(0.15)
 C31B(0.15) C32B(0.15) C30B(0.15) C22A(0.7) F3A(0.7) F2A(0.7) C24A(0.7)
 F9A(0.7) F8A(0.7) C23A(0.7) F6A(0.7) C24B(0.3) F8B(0.3) F9B(0.3) C23B(0.3)
 F6B(0.3) C22B(0.3) F3B(0.3) F2B(0.3) C34A(0.73) F30A(0.73) F29A(0.73)
 C35A(0.73) F32A(0.73) F33A(0.73) F31A(0.73) C34B(0.27) F30B(0.27) C36B(0.27)
 F35B(0.27) F36B(0.27) F34B(0.27) C35B(0.27) F32B(0.27) F33B(0.27) F31B(0.27)
 C36A(0.73) F36A(0.73) F34A(0.73) F35A(0.73) F29B(0.27)
5.a Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C9(H9A,H9B,H9C),
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C),
  C8(H8A,H8B,H8C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              90563
_shelx_hkl_checksum              73012
_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
;