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_1564639
_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 H37 As0.96 Fe0.96 P4.8, Al C16 F36 O4, 0.04(As Fe P5), 0.5[C7H8]'
_chemical_formula_sum            'C41.5 H41 Al As F36 Fe O4 P5'
_chemical_formula_weight         1600.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-18
_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                 113.8980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.0092(2)
_cell_length_b                   21.7375(2)
_cell_length_c                   10.53850(10)
_cell_measurement_reflns_used    38845
_cell_measurement_temperature    123.15(1)
_cell_measurement_theta_max      66.8470
_cell_measurement_theta_min      3.9860
_cell_volume                     5866.28(10)
_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(1)
_diffrn_detector_area_resol_mean 8.4094
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_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 -46.00   0.50    3.00    --  -43.66 103.00 -48.00   50
  2  \w     10.00  35.00   0.50    3.00    --   43.66-103.00-150.00   50
  3  \w     20.00  45.00   0.50   12.00    --   86.50-103.00-150.00   50
  4  \w     96.00 121.00   0.50   12.00    --   86.50 103.00 -48.00   50
  5  \w   -161.00-136.00   0.50   12.00    --  -90.00-103.00-150.00   50
  6  \w    -83.00 -58.00   0.50   12.00    --  -90.00 103.00 -48.00   50
  7  \w     39.00 115.00   0.50    3.00    --   43.66  37.00 -30.00  152
  8  \w     14.00  86.00   0.50    3.00    --   43.66-125.00  60.00  144
  9  \w      7.00  76.00   0.50    3.00    --   43.66-125.00-180.00  138
 10  \w   -155.00-128.00   0.50   12.00    --  -90.00-125.00  30.00   54
 11  \w   -104.00 -29.00   0.50   12.00    --  -90.00 125.00-150.00  150
 12  \w   -154.00 -98.00   0.50   12.00    --  -90.00-125.00 -60.00  112
 13  \w    -63.00 -36.00   0.50   12.00    --  -90.00  77.00 -60.00   54
 14  \w   -157.00-102.00   0.50   12.00    --  -90.00-125.00-120.00  110
 15  \w   -161.00-105.00   0.50   12.00    --  -90.00 -94.00 -30.00  112
 16  \w   -146.00-110.00   0.50   12.00    --  -90.00-125.00   0.00   72
 17  \w   -161.00-130.00   0.50   12.00    --  -90.00-135.00 146.63   62
 18  \w   -148.00-121.00   0.50   12.00    --  -90.00-125.00  60.00   54
 19  \w   -104.00 -35.00   0.50   12.00    --  -90.00 125.00 -60.00  138
 20  \w   -117.00 -73.00   0.50   12.00    --  -90.00  61.00 -60.00   88
 21  \w    -48.00 -20.00   0.50   12.00    --  -90.00  61.00 -60.00   56
 22  \w   -113.00 -57.00   0.50   12.00    --  -90.00  47.00 -58.47  112
 23  \w   -160.00-122.00   0.50   12.00    --  -90.00 -49.00  51.59   76
 24  \w   -102.00 -71.00   0.50   12.00    --  -90.00 -49.00  51.59   62
 25  \w    -78.00 -18.00   0.50   12.00    --  -90.00  30.00 -90.00  120
 26  \w    -84.00 -57.00   0.50   12.00    --  -90.00 125.00   0.00   54
 27  \w   -158.00-109.00   0.50   12.00    --  -90.00 -30.00-180.00   98
 28  \w    -88.00 -63.00   0.50   12.00    --  -90.00 -30.00-180.00   50
 29  \w   -120.00 -86.00   0.50   12.00    --  -90.00  77.00 -60.00   68
 30  \w   -124.00 -99.00   0.50   12.00    --  -90.00-135.00 146.63   50
 31  \w    -79.00 -52.00   0.50   12.00    --  -90.00  45.00  60.00   54
 32  \w   -145.00-116.00   0.50   12.00    --  -90.00 -57.00-138.11   58
 33  \w   -142.00-115.00   0.50   12.00    --  -90.00-125.00-150.00   54
 34  \w   -163.00-116.00   0.50   12.00    --  -90.00 -77.00-120.00   94
 35  \w    -87.00 -62.00   0.50   12.00    --  -90.00 125.00 -90.00   50
 36  \w   -110.00 -83.00   0.50   12.00    --  -90.00  61.00  30.00   54
 37  \w   -132.00-105.00   0.50   12.00    --  -90.00 -61.00  60.00   54
 38  \w   -137.00-110.00   0.50   12.00    --  -90.00 -77.00 -30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            61278
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.906
_diffrn_reflns_theta_max         66.906
_diffrn_reflns_theta_min         4.007
_exptl_absorpt_coefficient_mu    5.578
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.246
_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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_description       block
_exptl_crystal_F_000             3172
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.219
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1182
_refine_ls_number_reflns         10404
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+9.2937P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1429
_refine_ls_wR_factor_ref         0.1469
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9640
_reflns_number_total             10404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr723_cua_abs
_cod_original_formula_sum        'C41.50 H41 Al As F36 Fe O4 P5'
_cod_database_code               1564639
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.375
_shelx_estimated_absorpt_t_min   0.173
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All As(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17B-C18B \\sim C22B-C17B
 with sigma of 0.02
 P2B-P1B \\sim P5B-P1B \\sim P3B-P4B \\sim P3B-P2B \\sim P5B-P4B
 with sigma of 0.02
 P2B-P5B \\sim P2B-P4B \\sim P5B-P3B
 with sigma of 0.02
 C38A-C35A \\sim C38B-C35B \\sim C36A-C35A \\sim C36B-C35B \\sim C37A-C35A
\\sim C37B-C35B
 with sigma of 0.02
 C33B-C31 \\sim C33A-C31 \\sim C34B-C31 \\sim C34A-C31 \\sim C32B-C31 \\sim
C32A-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C30B \\sim C30A \\sim C27: within 1.9A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 1.9A
O1: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
1.7A
O4B \\sim O4A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C37B \\sim C37A \\sim C35B \\sim C35A \\sim C38B \\sim C38A \\sim C36B \\sim
C36A: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.9A
C23B \\sim C23A \\sim C25B \\sim C24A \\sim F1: within 1.9A with sigma of 0.01
and sigma for terminal atoms of 0.01 within 1.9A
C32A \\sim C32B \\sim C31 \\sim C34B \\sim C34A \\sim C33A \\sim C33B: within
1.9A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.9A
F17A \\sim F18A \\sim F16A \\sim C30A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
F18B \\sim F16B \\sim C30B \\sim F17B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
F21B \\sim C32B \\sim F19B \\sim F20B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
F22B \\sim F23B \\sim F24B \\sim C33B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
F9 \\sim C26 \\sim F7 \\sim F8: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.9A
F34B \\sim C38B \\sim F35B: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.9A
4. Others
 Fixed Sof: Fe1A(0.96) P1A(0.96) P2A(0.96) P5A(0.96) P4A(0.96) P3A(0.96)
 O2A(0.5) F20A(0.7) F32A(0.7) O3A(0.7) F33A(0.7) O4A(0.7) F25A(0.7) F23A(0.7)
 F30A(0.7) F21A(0.7) F29A(0.7) F35A(0.7) F19A(0.7) F16A(0.5) C35A(0.7)
 F22A(0.7) F6A(0.69) F5A(0.69) F3A(0.69) F26A(0.7) F31A(0.7) F18A(0.5)
 F4A(0.69) F34A(0.7) F17A(0.5) F24A(0.7) C17A(0.56) H17A(0.56) H20A(0.56)
 H20B(0.56) H20C(0.44) H20D(0.44) C25A(0.69) C37A(0.7) C32A(0.7) C23A(0.69)
 C30A(0.5) C34A(0.7) C38A(0.7) C36A(0.7) C24A(0.69) C33A(0.7) C22A(0.56)
 H22A(0.56) H22B(0.56) C21A(0.56) H21A(0.56) H21B(0.56) C18A(0.56) H18A(0.56)
 H18B(0.56) C19A(0.56) H19A(0.56) H19B(0.56) F28A(0.7) F4B(0.31) F3B(0.31)
 F5B(0.31) C25B(0.31) C23B(0.31) C24B(0.31) F6B(0.31) F32B(0.3) F30B(0.3)
 F29B(0.3) F35B(0.3) C35B(0.3) F31B(0.3) F34B(0.3) C37B(0.3) C38B(0.3)
 C36B(0.3) F28B(0.3) F33B(0.3) F20B(0.3) F25B(0.3) F23B(0.3) F21B(0.3)
 F19B(0.3) F22B(0.3) F26B(0.3) F24B(0.3) C32B(0.3) C34B(0.3) C33B(0.3)
 F16B(0.5) F18B(0.5) F17B(0.5) C30B(0.5) O4B(0.3) O3B(0.3) O2B(0.5) C17B(0.44)
 C18B(0.44) H18C(0.44) H18D(0.44) C19B(0.44) H19C(0.44) H19D(0.44) C22B(0.44)
 H22C(0.44) H22D(0.44) C21B(0.44) H21C(0.44) H21D(0.44) As1B(0.04) Fe1B(0.04)
 P1B(0.04) P2B(0.04) P5B(0.04) P3B(0.04) P4B(0.04) As1A(0.96) H17B(0.44)
 Fixed Uiso: As1B(0.05) Fe1B(0.05) P1B(0.05) P2B(0.05) P5B(0.05) P3B(0.05)
 P4B(0.05)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C17A(H17A)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C15(H15A,H15B), C16(H16A,H16B), C14(H14A,H14B), C13(H13A,
 H13B), C20(H20A,H20B), C20(H20C,H20D), C22A(H22A,H22B), C21A(H21A,H21B),
 C18A(H18A,H18B), C19A(H19A,H19B), C18B(H18C,H18D), C19B(H19C,H19D), C22B(H22C,
 H22D), C21B(H21C,H21D)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C),
 C8(H8A,H8B,H8C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 98 electrons were 
found in a volume of 344\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.5[C7H8] per Asymmetric Unit 
which account for 100 electrons 
per unit cell.
;
_shelx_res_checksum              14567
_shelx_hkl_checksum              76244
_shelx_fab_checksum              79089
_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
;