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_1564646
_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         'C16 H20 Fe P5 Se, Al C16 F36 O4'
_chemical_formula_sum            'C32 H20 Al F36 Fe O4 P5 Se'
_chemical_formula_weight         1469.12
_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             2021-03-19
_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                107.670(4)
_cell_angle_beta                 96.922(3)
_cell_angle_gamma                90.247(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1286(4)
_cell_length_b                   12.6674(5)
_cell_length_c                   17.2846(8)
_cell_measurement_reflns_used    7948
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      31.3100
_cell_measurement_theta_min      3.8960
_cell_volume                     2509.49(18)
_computing_cell_refinement       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.869
_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    -92.00  11.00   1.00    6.34    --  -18.24 -57.00  90.00  103
  2  \w    -91.00  14.00   1.00    6.34    --  -18.24 -77.00 -30.00  105
  3  \w    -44.00  47.00   1.00    6.34    --  -18.24  57.00-120.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22005
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.286
_diffrn_reflns_theta_min         3.379
_exptl_absorpt_coefficient_mu    1.374
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.27a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.944
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.436
_exptl_crystal_size_min          0.277
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         15499
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0528P)^2^+0.7646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11637
_reflns_number_total             15499
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr346_mo
_cod_database_code               1564646
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.702
_shelx_estimated_absorpt_t_min   0.537
_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
 F29A-C30A \\sim F29B-C30B \\sim F30A-C30A \\sim F30B-C30B \\sim F28-C30A
 with sigma of 0.02
 C31B-C29 \\sim C31A-C29 \\sim C32A-C29 \\sim C32B-C29 \\sim C30A-C29 \\sim
C30B-C29
 with sigma of 0.02
 F35A-C32A \\sim F36-C32A \\sim F35B-C32B \\sim F34-C32B \\sim F34-C32A
 with sigma of 0.02
 F32B-C31B \\sim F33A-C31A \\sim F33B-C31B \\sim F31-C31B \\sim F31-C31A \\sim
F32A-C31A
 with sigma of 0.02
 F34-F36 \\sim F36-F35B \\sim F35B-F34
 with sigma of 0.02
 F27B-C28B \\sim F26B-C28B \\sim F25-C28B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C32B \\sim C30B \\sim C29 \\sim C31B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
C32B \\sim F35B: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.005 within 1.9A
C31B \\sim F32B \\sim F33B: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F36: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.01 within
1.9A
F16B \\sim C24 \\sim F18B \\sim F17B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
F27B \\sim C28B \\sim F26B \\sim C28A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
F29B \\sim C30B \\sim F30B: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F24B \\sim F23B \\sim C27: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
4. Others
 Fixed Sof: F27A(0.86) F23A(0.86) F21A(0.86) F24A(0.86) F26A(0.86) F20A(0.86)
 F16A(0.74) F18A(0.74) F11A(0.74) F12A(0.74) F15B(0.74) F17A(0.74) F14B(0.74)
 C28A(0.86) F24B(0.14) F23B(0.14) F21B(0.14) F20B(0.14) F27B(0.14) C28B(0.14)
 F26B(0.14) F11B(0.26) F12B(0.26) F14A(0.26) F15A(0.26) F17B(0.26) F18B(0.26)
 F16B(0.26) C31A(0.91) C32A(0.91) C30A(0.91) F33A(0.91) F35A(0.91) F32A(0.91)
 F30A(0.91) F29A(0.91) C31B(0.09) F33B(0.09) F32B(0.09) C32B(0.09) F35B(0.09)
 F29B(0.09) C30B(0.09) F30B(0.09)
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C5(H5), C4(H4), C3(H3)
5.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C14(H14A,H14B,H14C), C13(H13A,H13B,
 H13C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              48059
_shelx_hkl_checksum              16565
_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
;