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_1564645
_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         'C17 H22 Fe P5, Al C16 F36 O4'
_chemical_formula_sum            'C33 H22 Al F36 Fe O4 P5'
_chemical_formula_weight         1404.18
_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   geom
_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                90
_cell_angle_beta                 106.706(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0993(7)
_cell_length_b                   18.0632(8)
_cell_length_c                   18.8351(10)
_cell_measurement_reflns_used    10149
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.3840
_cell_measurement_theta_min      2.9550
_cell_volume                     4920.3(4)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.947
_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    -44.00  10.00   1.00   15.00    --  -44.33  57.00 -60.00   54
  2  \w   -107.00  19.00   1.00   15.00    --  -44.33   0.00  90.00  126
  3  \w     35.00  93.00   1.00   60.00    --  104.50 -61.00  90.00   58
  4  \w     43.00  93.00   1.00   60.00    --  104.50 -61.00 -90.00   50
  5  \w     86.00 173.00   1.00   60.00    --  104.50  45.00-120.00   87
  6  \w     42.00 111.00   1.00   60.00    --  104.50-125.00  60.00   69
  7  \w     35.00  93.00   1.00   60.00    --  104.50 -61.00  30.00   58
  8  \w     36.00  72.00   1.00   60.00    --  104.50 -45.00 120.00   36
  9  \w     36.00  72.00   1.00   60.00    --  104.50 -45.00 150.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0785069000
_diffrn_orient_matrix_UB_12      -0.0217332000
_diffrn_orient_matrix_UB_13      -0.0191210000
_diffrn_orient_matrix_UB_21      0.0543590000
_diffrn_orient_matrix_UB_22      0.0156533000
_diffrn_orient_matrix_UB_23      0.0716068000
_diffrn_orient_matrix_UB_31      -0.0118959000
_diffrn_orient_matrix_UB_32      -0.0723769000
_diffrn_orient_matrix_UB_33      0.0213204000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26352
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         75.377
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50(Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.279
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.436
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.27a (Rigaku Oxford Diffraction, 2019)
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    1.896
_exptl_crystal_description       block
_exptl_crystal_F_000             2760
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1385
_refine_ls_number_reflns         13101
_refine_ls_number_restraints     608
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0703P)^2^+4.0464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1462
_refine_ls_wR_factor_ref         0.1640
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10904
_reflns_number_total             13101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr451_cub
_cod_database_code               1564645
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C156 H180 Al4 F92 Fe4 O44 P20 '
_shelx_estimated_absorpt_t_max   0.494
_shelx_estimated_absorpt_t_min   0.343
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.15
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Al1-O3A \\sim Al1-O3B
 with sigma of 0.02
 C21A-C18 \\sim C21B-C18 \\sim C20B-C18 \\sim C20A-C18 \\sim C19-C18
 with sigma of 0.02
 F26B-C29B \\sim F25B-C29B \\sim F25C-C29C \\sim F27C-C29C \\sim F26C-C29C
\\sim F27B-C29B
 with sigma of 0.02
 C9B-C8B \\sim C9A-C8A \\sim C12A-C8A \\sim C12B-C8B \\sim C11B-C12B \\sim
C11A-C12A \\sim C10A-C11A ~
 C11B-C10B \\sim C10A-C9A \\sim C10B-C9B
 with sigma of 0.02
 F20B-C27B \\sim F19B-C27B \\sim F21B-C27B \\sim F21C-C27C \\sim F19C-C27C
\\sim F20C-C27C
 with sigma of 0.02
 F24A-C28A \\sim F23A-C28A \\sim F22A-C28A
 with sigma of 0.02
 F14B-C24 \\sim F14A-C24 \\sim F15B-C24 \\sim F15A-C24
 with sigma of 0.02
 F31A-C32A \\sim F33A-C32A \\sim F32A-C32A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C29A \\sim C29C \\sim C29B \\sim C26 \\sim C28B \\sim C28C \\sim C28A \\sim
C27B \\sim C27C \\sim C27A: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
C33B \\sim C33A \\sim C30 \\sim C31B \\sim C31A \\sim C32B \\sim C32A: within
1.9A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.9A
F21C \\sim C27C \\sim F20A: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
C29B \\sim C29C \\sim F25C \\sim F25B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
C21A \\sim C21B \\sim F7A \\sim F7B \\sim F8A \\sim F8B \\sim F9B \\sim F9A:
within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.9A
C7B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C1B: within 1.9A
with sigma of 0.005 and sigma for terminal atoms of 0.02 within 1.9A
C10B \\sim C16B \\sim C11B \\sim C15B \\sim C9B \\sim C14B \\sim C8B \\sim C13B
\\sim C12B \\sim C17B \\sim C12A: within 1.9A with sigma of 0.005 and sigma for
terminal atoms of 0.02 within 1.9A
C24 \\sim F13: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.9A
F15B \\sim F15A \\sim C24: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F22C \\sim C28C \\sim F24C \\sim F23C: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
4. Others
 Fixed Sof: P5A(0.93) P4A(0.93) P1A(0.93) P3A(0.93) P2A(0.93) F16A(0.75)
 F32B(0.75) F15A(0.75) F14A(0.75) F17A(0.75) F18A(0.75) F8A(0.71) F31B(0.75)
 F33B(0.75) F7A(0.71) C8A(0.68) F4A(0.71) C12A(0.68) F6A(0.71) F9A(0.71)
 F5A(0.71) C9A(0.68) C2A(0.93) C11A(0.68) C25A(0.75) C3A(0.93) H3A(0.93)
 C32B(0.75) C10A(0.68) C7A(0.93) H7A(0.93) C13A(0.68) H13A(0.68) H13B(0.68)
 H13C(0.68) C1A(0.93) H1AA(0.93) H1AB(0.93) C21A(0.71) C17A(0.68) H17A(0.68)
 H17B(0.68) H17C(0.68) C20A(0.71) C4A(0.93) H4A(0.93) C16A(0.68) H16A(0.68)
 H16B(0.68) H16C(0.68) C15A(0.68) H15A(0.68) H15B(0.68) H15C(0.68) C14A(0.68)
 H14A(0.68) H14B(0.68) H14C(0.68) C5A(0.93) H5A(0.93) C6A(0.93) H6A(0.93)
 F31A(0.25) F36A(0.25) F35A(0.25) F33A(0.25) F32A(0.25) F34A(0.25) F30A(0.25)
 F28A(0.25) F29A(0.25) C33A(0.25) C32A(0.25) C31A(0.25) O3A(0.73) F20B(0.37)
 F23B(0.37) F26B(0.37) F25B(0.37) F22B(0.37) F19B(0.37) C27A(0.24) F24B(0.37)
 C29B(0.37) C28B(0.37) F21B(0.37) F27B(0.37) O3B(0.27) F20A(0.24) F23A(0.24)
 F26A(0.24) F25A(0.24) F22A(0.24) F19A(0.24) F24A(0.24) C29A(0.24) C28A(0.24)
 F21A(0.24) F27A(0.24) C27B(0.37) C28C(0.39) F24C(0.39) F23C(0.39) F22C(0.39)
 F21C(0.39) C27C(0.39) F20C(0.39) F19C(0.39) C29C(0.39) F27C(0.39) F25C(0.39)
 F26C(0.39) C8B(0.32) C12B(0.32) C9B(0.32) C11B(0.32) C10B(0.32) C13B(0.32)
 H13D(0.32) H13E(0.32) H13F(0.32) C17B(0.32) H17D(0.32) H17E(0.32) H17F(0.32)
 C16B(0.32) H16D(0.32) H16E(0.32) H16F(0.32) C15B(0.32) H15D(0.32) H15E(0.32)
 H15F(0.32) C14B(0.32) H14D(0.32) H14E(0.32) H14F(0.32) P1B(0.07) P2B(0.07)
 P5B(0.07) P4B(0.07) P3B(0.07) F16B(0.25) F15B(0.25) F14B(0.25) F17B(0.25)
 F18B(0.25) C25B(0.25) F8B(0.29) F7B(0.29) F4B(0.29) F6B(0.29) F9B(0.29)
 F5B(0.29) C21B(0.29) C20B(0.29) F36B(0.75) F35B(0.75) F34B(0.75) F29B(0.75)
 F30B(0.75) F28B(0.75) C33B(0.75) C31B(0.75) C1B(0.07) H1BA(0.07) H1BB(0.07)
 C2B(0.07) C7B(0.07) H7B(0.07) C6B(0.07) H6B(0.07) C5B(0.07) H5B(0.07)
 C4B(0.07) H4B(0.07) C3B(0.07) H3B(0.07) O4B(0.75) O4A(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C1A(H1AA,H1AB), C1B(H1BA,H1BB)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C7A(H7A), C4A(H4A), C5A(H5A), C6A(H6A), C7B(H7B), C6B(H6B),
 C5B(H5B), C4B(H4B), C3B(H3B)
5.c Fitted hexagon refined as free rotating group:
 C2B(C7B,C6B,C5B,C4B,C3B)
5.d Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C17A(H17A,H17B,H17C), C16A(H16A,H16B,H16C), C15A(H15A,
 H15B,H15C), C14A(H14A,H14B,H14C), C13B(H13D,H13E,H13F), C17B(H17D,H17E,H17F),
 C16B(H16D,H16E,H16F), C15B(H15D,H15E,H15F), C14B(H14D,H14E,H14F)
;
_shelx_res_checksum              86208
_shelx_hkl_checksum              19830
_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 1.346
_oxdiff_exptl_absorpt_empirical_full_min 0.728