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_1564643
_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
'2(C17 H27 I Sb), 2(C10 H15 Fe P5), 2(Al C16 F36 O4), 0.5[C6H14], 0.5[C6H14]'
_chemical_formula_sum            'C92 H98 Al2 F72 Fe2 I2 O8 P10 Sb2'
_chemical_formula_weight         3672.36
_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             2021-03-19
_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                90
_cell_angle_beta                 92.2010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0539(2)
_cell_length_b                   16.5834(2)
_cell_length_c                   38.0631(4)
_cell_measurement_reflns_used    17655
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.1720
_cell_measurement_theta_min      4.1850
_cell_volume                     13279.7(2)
_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_temperature      123(1)
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.971
_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    -98.00 -18.00   1.00   10.00    --  -39.78 125.00 -90.00   80
  2  \w    -43.00  27.00   1.00   10.00    --   39.78 -19.00 -90.00   70
  3  \w    -43.00  27.00   1.00   10.00    --   39.78 -19.00 -30.00   70
  4  \w    -38.00  43.00   1.00   10.00    --   39.78 -38.00  30.00   81
  5  \w     15.00 178.00   1.00   40.00    --  105.16   0.00-120.00  163
  6  \w     21.00 141.00   1.00   40.00    --  105.16 -82.00 -68.06  120
  7  \w     76.00 178.00   1.00   40.00    --  105.16  45.00-120.00  102
  8  \w     21.00 141.00   1.00   40.00    --  105.16 -81.00  87.79  120
  9  \w   -121.00  -5.00   1.00   10.00    --  -39.78 -77.00  90.00  116
 10  \w      9.00 116.00   1.00   10.00    --   39.78  57.00   0.00  107
 11  \w     28.00 111.00   1.00   40.00    --  105.16  15.00  60.00   83
;
_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  0.0782
_diffrn_reflns_av_unetI/netI     0.0814
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            75069
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.750
_diffrn_reflns_theta_min         3.394
_exptl_absorpt_coefficient_mu    11.213
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.070
_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            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       rod
_exptl_crystal_F_000             7192
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.083
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2570
_refine_ls_number_reflns         25253
_refine_ls_number_restraints     1318
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0649
_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^)+(0.0761P)^2^+34.5007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1737
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18923
_reflns_number_total             25253
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04296c2.cif
_cod_data_source_block           cr379_cua
_cod_database_code               1564643
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.456
_shelx_estimated_absorpt_t_min   0.066
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C55A-F2A \\sim C55A-F1A \\sim C55A-F3A
 with sigma of 0.02
 C70-C73B \\sim C70-C71B \\sim C70-C72
 with sigma of 0.02
 C84C-C82 \\sim C82-C84A \\sim C84B-C82 \\sim C82-C83A \\sim C83B-C82 \\sim
C83C-C82 \\sim C85B-C82 ~
 C82-C85A \\sim C85C-C82
 with sigma of 0.02
 C53B-C44B \\sim C53B-C47B \\sim C49B-C48B \\sim C49B-C45B \\sim C50B-C44B
\\sim C50B-C46B \\sim C51B-
 C45B \\sim C51B-C47B \\sim C52B-C46B \\sim C52B-C48B
 with sigma of 0.04
 C81B-C78 \\sim C81A-C78
 with sigma of 0.02
 F58-C80B \\sim F58-C80A \\sim F59B-C80B \\sim F59A-C80A \\sim F60B-C80B \\sim
F60A-C80A
 with sigma of 0.02
 C48B-C53B \\sim C44B-C49B \\sim C45B-C50B \\sim C46B-C51B \\sim C47B-C52B
 with sigma of 0.04
 F49C-C76B \\sim F51B-C76B \\sim F50B-C76B
 with sigma of 0.02
 C80B-C78 \\sim C80A-C78
 with sigma of 0.02
 C76A-C74 \\sim C76B-C74
 with sigma of 0.02
 F61B-C81B \\sim F62B-C81B \\sim F63B-C81B
 with sigma of 0.02
 C48B-C44B \\sim C44B-C45B \\sim C45B-C46B \\sim C46B-C47B \\sim C47B-C48B
 with sigma of 0.04
 F13B-F15B \\sim F15B-F14B \\sim F14B-F13B
 with sigma of 0.02
 F8A-C57A \\sim F7A-C57A \\sim F9A-C57A
 with sigma of 0.02
 C57B-C54B \\sim C57A-C54A \\sim C56A-C54A \\sim C56B-C54B \\sim C55B-C54B
\\sim C55A-C54A
 with sigma of 0.02
 F24B-C64B \\sim F22B-C64B \\sim F23B-C64B
 with sigma of 0.02
 F12B-C59B \\sim F10-C59B \\sim F11B-C59B
 with sigma of 0.02
 F10-F11B \\sim F11B-F12B \\sim F12B-F10
 with sigma of 0.02
 C65B-F27B \\sim C65B-F25B \\sim C65B-F26B
 with sigma of 0.02
 C63B-F19B \\sim C63B-F20B \\sim C63B-F21B
 with sigma of 0.02
 F27B-F25B \\sim F25B-F26B \\sim F26B-F27B
 with sigma of 0.02
 F24B-F22B \\sim F22B-F23B \\sim F23B-F24B
 with sigma of 0.02
 F19B-F20B \\sim F20B-F21B \\sim F21B-F19B
 with sigma of 0.02
 C63A-C62A \\sim C62B-C63B \\sim C65B-C62B \\sim C65A-C62A \\sim C64B-C62B
\\sim C64A-C62A
 with sigma of 0.02
 C65B-C64B \\sim C64B-C63B \\sim C63B-C65B
 with sigma of 0.02
 O3B-C62B \\sim O3A-C62A
 with sigma of 0.02
 C12A-C10 \\sim C12B-C10 \\sim C13A-C10 \\sim C13B-C10 \\sim C10-C11
 with sigma of 0.02
 F9B-C57B \\sim F7B-C57B \\sim F8B-C57B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F39A \\sim F37A \\sim F38B \\sim C71A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C70 \\sim C73B \\sim C71B \\sim C72 \\sim C71A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
F39B \\sim F38B \\sim F37B \\sim C71B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F45A \\sim F43A \\sim F44A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F43B \\sim C73B \\sim F45B \\sim F44B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C82 \\sim C85B \\sim C85A \\sim C85C \\sim C83A \\sim C83C \\sim C83B \\sim
C84B \\sim C84A \\sim C84C: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F68C \\sim F69C \\sim C84C: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
C76B \\sim F50B \\sim F51B \\sim C74: within 1.9A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 1.9A
C59B \\sim C58B \\sim C61 \\sim C60B \\sim C58A: within 1.9A with sigma of 0.01
and sigma for terminal atoms of 0.01 within 1.9A
C50A \\sim C45A \\sim C46A \\sim C51A \\sim C47A \\sim C52A \\sim C48A \\sim
C53A \\sim C44A \\sim C49A \\sim C50B \\sim C45B \\sim C51B \\sim C46B \\sim
C47B \\sim C52B \\sim C48B \\sim C53B \\sim C44B \\sim C49B: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
F13B \\sim C60B \\sim F14B \\sim F15B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
C55B \\sim F2B \\sim F3B \\sim F1B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
C81A \\sim C81B \\sim F61B \\sim F62B \\sim F63B: within 1.9A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.9A
C80B \\sim C80A: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.9A
F1A \\sim C55A \\sim F2A \\sim F3A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.005 within 1.9A
F53A \\sim F53B \\sim C77A \\sim C77B \\sim F54A \\sim F54B: within 1.9A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.9A
C57A \\sim F7A \\sim F9A \\sim F8A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
O8B \\sim O8A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F71B \\sim C85A \\sim F72A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C54B \\sim C54A \\sim C55B \\sim C55A \\sim C56B \\sim C56A \\sim C57B \\sim
C57A: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.9A
F12B \\sim C59B \\sim F11B: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
C65B \\sim C62B \\sim C62A \\sim C64B \\sim C63B \\sim C63A \\sim C64A \\sim
C65A: within 1.9A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.9A
C63B \\sim F20B \\sim F19B \\sim F21B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
F25B \\sim C65B \\sim F26B \\sim F27B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
C64B \\sim F22B \\sim F23B \\sim F24B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
O3A \\sim O3B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C12B \\sim C13B \\sim C10 \\sim C2: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.005 within 1.9A
O4B \\sim O4A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C40 \\sim C35: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C43 \\sim C38: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C38 \\sim C43: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C44 \\sim C39: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F4B \\sim C56B \\sim F6B \\sim F5B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
F6A \\sim C56A \\sim F4A \\sim F5A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
C57B \\sim F8B \\sim F9B \\sim F7B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
C85C \\sim F70C: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
F65B \\sim C83B \\sim F64B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O5 \\sim O5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4. Others
 Fixed Sof: I2A(0.75) I1A(0.75) O5(0.5) F54A(0.74) O4A(0.47) F51A(0.74)
 F15A(0.68) O7A(0.67) F34A(0.47) F39B(0.5) F61A(0.67) F37B(0.5) F50A(0.74)
 F60A(0.67) F53A(0.74) F62A(0.67) O3A(0.67) F33A(0.47) F32A(0.47) F59A(0.67)
 F52A(0.74) F67A(0.68) F27A(0.67) F66A(0.73) F63A(0.67) C62A(0.67) F22A(0.67)
 F71A(0.41) F26A(0.67) F12A(0.68) F13A(0.68) F11A(0.68) F20A(0.67) F23A(0.67)
 F36A(0.47) F70A(0.73) F68A(0.41) F25A(0.67) F14A(0.68) F24A(0.67) F19A(0.67)
 C76A(0.74) C77A(0.74) F21A(0.67) C71B(0.5) C81A(0.67) C60A(0.68) F69A(0.41)
 C85A(0.41) C84A(0.41) C58A(0.68) C83A(0.41) C65A(0.67) C13A(0.75) H13A(0.75)
 H13B(0.75) H13C(0.75) F65A(0.41) C64A(0.67) C59A(0.68) C12A(0.75) H12A(0.75)
 H12B(0.75) H12C(0.75) C63A(0.67) F72A(0.41) C54A(0.59) C57A(0.59) C56A(0.59)
 F2A(0.59) F1A(0.59) F5A(0.59) F6A(0.59) F3A(0.59) F7A(0.59) F4A(0.59)
 F8A(0.59) F9A(0.59) C55A(0.59) I1B(0.25) I2B(0.25) C54B(0.41) C57B(0.41)
 F2B(0.41) F1B(0.41) F5B(0.41) F6B(0.41) F3B(0.41) F7B(0.41) F4B(0.41)
 F8B(0.41) F9B(0.41) C55B(0.41) C56B(0.41) F13B(0.32) F15B(0.32) F11B(0.32)
 F14B(0.32) F12B(0.32) C59B(0.32) C58B(0.32) C60B(0.32) F27B(0.33) F24B(0.33)
 F25B(0.33) F22B(0.33) F23B(0.33) F19B(0.33) F26B(0.33) F20B(0.33) F21B(0.33)
 C65B(0.33) C64B(0.33) C63B(0.33) F35A(0.47) C62B(0.33) F35B(0.53) F34B(0.53)
 F36B(0.53) F32B(0.53) F33B(0.53) F72B(0.59) F64B(0.32) F67B(0.32) F68B(0.32)
 F69B(0.32) C85B(0.32) C84B(0.32) C83B(0.32) F65B(0.32) F71B(0.32) F64A(0.68)
 F66C(0.27) F70C(0.27) F68C(0.27) F69C(0.27) C85C(0.27) C84C(0.27) C83C(0.27)
 F65C(0.27) F71C(0.27) C44A(0.7) C48A(0.7) C46A(0.7) C47A(0.7) C45A(0.7)
 C52A(0.7) H52A(0.7) H52B(0.7) H52C(0.7) C53A(0.7) H53A(0.7) H53B(0.7)
 H53C(0.7) C49A(0.7) H49A(0.7) H49B(0.7) H49C(0.7) C51A(0.7) H51A(0.7)
 H51B(0.7) H51C(0.7) C50A(0.7) H50A(0.7) H50B(0.7) H50C(0.7) O3B(0.33)
 O4B(0.53) O8B(0.35) O8A(0.65) O7B(0.33) F61B(0.33) F62B(0.33) F63B(0.33)
 C80A(0.67) C81B(0.33) C13B(0.25) H13D(0.25) H13E(0.25) H13F(0.25) C12B(0.25)
 H12D(0.25) H12E(0.25) H12F(0.25) F54B(0.26) F51B(0.26) F50B(0.26) F53B(0.26)
 F52B(0.26) C76B(0.26) C77B(0.26) F38B(0.5) F43B(0.5) F44B(0.5) F45B(0.5)
 C73B(0.5) F59B(0.33) F60B(0.33) C80B(0.33) C48B(0.3) C44B(0.3) C45B(0.3)
 C46B(0.3) C47B(0.3) C52B(0.3) H52D(0.3) H52E(0.3) H52F(0.3) C51B(0.3)
 H51D(0.3) H51E(0.3) H51F(0.3) C50B(0.3) H50D(0.3) H50E(0.3) H50F(0.3)
 C49B(0.3) H49D(0.3) H49E(0.3) H49F(0.3) C53B(0.3) H53D(0.3) H53E(0.3)
 H53F(0.3) C71A(0.5) F37A(0.5) F38A(0.5) F39A(0.5) F44A(0.5) C73A(0.5)
 F43A(0.5) F45A(0.5) O5A(0.5)
 Fixed X: F42(0.232029)
 Fixed Y: F42(0.47026)
 Fixed Z: F42(0.381881)
5.a Idealised Me refined with riding coordinates:
 C52A(H52A,H52B,H52C), C53A(H53A,H53B,H53C), C49A(H49A,H49B,H49C), C51A(H51A,
 H51B,H51C), C50A(H50A,H50B,H50C), C52B(H52D,H52E,H52F), C51B(H51D,H51E,H51F),
 C50B(H50D,H50E,H50F), C49B(H49D,H49E,H49F), C53B(H53D,H53E,H53F)
5.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C34(H34A,H34B,
 H34C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C24(H24A,H24B,H24C), C33(H33A,
 H33B,H33C), C32(H32A,H32B,H32C), C15(H15A,H15B,H15C), C41(H41A,H41B,H41C),
 C17(H17A,H17B,H17C), C7(H7A,H7B,H7C), C26(H26A,H26B,H26C), C8(H8A,H8B,H8C),
 C44(H44A,H44B,H44C), C42(H42A,H42B,H42C), C40(H40A,H40B,H40C), C9(H9A,H9B,H9C),
  C43(H43A,H43B,H43C), C13A(H13A,H13B,H13C), C12A(H12A,H12B,H12C), C11(H11A,
 H11B,H11C), C13B(H13D,H13E,H13F), C12B(H12D,H12E,H12F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 204 electrons were 
found in a volume of 1206\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.5[C6H14], 0.5[C6H14] per Asymmetric Unit 
which account for 200 electrons 
per unit cell.
;
_shelx_res_checksum              3816
_shelx_hkl_checksum              30786
_shelx_fab_checksum              71276
_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
;