Teaching old tricks to new dogs - rational synthesis of multi-decker complexes featuring <i>cyclo</i>-P<sub>5</sub> decks.
Riesinger, Christoph; Röhner, David; Krossing, Ingo; Scheer, Manfred; Chemical communications (Cambridge, England) 59 (2023) 4495–4498; doi:10.1039/d3cc00898c

data_7131455
_publ_section_title
;
 Teaching old tricks to new dogs - rational synthesis of multi-decker
 complexes featuring <i>cyclo</i>-P<sub>5</sub> decks.
;
_journal_issue                   30
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4495
_journal_page_last               4498
_journal_paper_doi               10.1039/d3cc00898c
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety
'C20 H30 As10 Fe3, 2(Al C16 F36 O4), 3(C6 H4 F2)'
_chemical_formula_sum            'C70 H42 Al2 As10 F78 Fe3 O8'
_chemical_formula_weight         3463.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-23
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-03-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.8080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.7409(2)
_cell_length_b                   14.01600(10)
_cell_length_c                   22.6687(2)
_cell_measurement_reflns_used    41734
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      71.4970
_cell_measurement_theta_min      2.6530
_cell_volume                     10453.57(14)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.977
_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     21.00  72.00   0.50    0.35    --   60.79 -95.00-180.00  102
  2  \w     19.00  90.00   0.50    0.35    --   60.79-125.00 -30.00  142
  3  \w     31.00  76.00   0.50    0.35    --   74.37-125.00  30.00   90
  4  \w     21.00  72.00   0.50    0.35    --   60.79 -95.00  90.00  102
  5  \w     21.00  72.00   0.50    0.35    --   60.79 -95.00  30.00  102
  6  \w     35.00  85.00   0.50    0.35    --   74.37 -95.00 -60.00  100
  7  \w     11.00  40.00   0.50    0.35    --   60.79 -30.00-150.00   58
  8  \w     11.00  40.00   0.50    0.35    --   60.79 -30.00-180.00   58
  9  \w   -111.00 -62.00   0.50    0.35    --  -61.39 -30.00 -60.00   98
 10  \w   -125.00 -76.00   0.50    0.35    --  -75.28 -30.00 -90.00   98
 11  \w   -111.00 -62.00   0.50    0.35    --  -61.39 -30.00-150.00   98
 12  \w   -124.00 -76.00   0.50    0.35    --  -74.96 -30.00-180.00   96
 13  \w   -125.00 -76.00   0.50    0.35    --  -75.28 -30.00-120.00   98
 14  \w   -108.00 -28.00   0.50    0.35    --  -61.39 -15.00  30.00  160
 15  \w   -124.00 -76.00   0.50    0.35    --  -74.96 -30.00   0.00   96
 16  \w   -122.00 -42.00   0.50    0.35    --  -75.28 -15.00  30.00  160
 17  \w   -124.00 -76.00   0.50    0.35    --  -74.96 -30.00 120.00   96
 18  \w   -119.00 -73.00   0.50    0.35    --  -74.96-125.00  30.00   92
 19  \w   -119.00 -73.00   0.50    0.35    --  -75.28-125.00-120.00   92
 20  \w   -104.00 -31.00   0.50    0.35    --  -75.28 125.00-150.00  146
 21  \w   -104.00 -31.00   0.50    0.35    --  -75.28 125.00  60.00  146
 22  \w   -101.00 -22.00   0.50    0.35    --  -61.39   0.00 120.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0254629000
_diffrn_orient_matrix_UB_12      -0.0277597000
_diffrn_orient_matrix_UB_13      0.0460269000
_diffrn_orient_matrix_UB_21      -0.0376779000
_diffrn_orient_matrix_UB_22      0.0469317000
_diffrn_orient_matrix_UB_23      -0.0404216000
_diffrn_orient_matrix_UB_31      -0.0111877000
_diffrn_orient_matrix_UB_32      -0.0953553000
_diffrn_orient_matrix_UB_33      -0.0333089000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            103420
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.908
_diffrn_reflns_theta_min         2.686
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.760
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.324
_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 green'
_exptl_crystal_density_diffrn    2.201
_exptl_crystal_description       block
_exptl_crystal_F_000             6648
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2363
_refine_ls_number_reflns         20045
_refine_ls_number_restraints     1584
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+7.8326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16042
_reflns_number_total             20045
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00898c2.cif
_cod_data_source_block           cr1168
_cod_depositor_comments
'Adding full bibliography for 7131448--7131455.cif.'
_cod_database_code               7131455
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C70H42O8F78Al2Fe3As10
_chemical_oxdiff_usercomment     Tian_Koenig_TYM-211105-a-4
_shelx_estimated_absorpt_t_max   0.579
_shelx_estimated_absorpt_t_min   0.287
_olex2_refinement_description
;
1. Restrained distances
 F35-C79 = F69-C79 = F75-C79 = F37-C5 = F19-C5 = F71-C5 = F77-C81 = F73-C81
 1.33 with sigma of 0.02
 F43-C21 = F85-C21 = F45-C21 = F89-C83 = F87-C83 = F21-C83 = F11-C41 = F83-C41
 = F41-C41
 1.33 with sigma of 0.02
 F59-C97 = F15-C97 = F61-C97
 1.33 with sigma of 0.02
 O9-C85
 1.4 with sigma of 0.02
 C21-C83
 2.55 with sigma of 0.04
 C41-C21
 2.55 with sigma of 0.04
 F77-F73
 2.2 with sigma of 0.04
 F35-F69
 2.2 with sigma of 0.04
 F69-F75
 2.2 with sigma of 0.04
 F75-F35
 2.2 with sigma of 0.04
 F37-F71
 2.2 with sigma of 0.04
 F71-F19
 2.2 with sigma of 0.04
 F19-F37
 2.2 with sigma of 0.04
 C83-C41
 2.55 with sigma of 0.04
 F43-F45
 2.2 with sigma of 0.04
 F45-F85
 2.2 with sigma of 0.04
 F85-F43
 2.2 with sigma of 0.04
 F89-F87
 2.2 with sigma of 0.04
 F87-F21
 2.2 with sigma of 0.04
 F21-F89
 2.2 with sigma of 0.04
 F11-F83
 2.2 with sigma of 0.04
 F83-F41
 2.2 with sigma of 0.04
 F41-F11
 2.2 with sigma of 0.04
 F59-F15
 2.2 with sigma of 0.04
 F15-F61
 2.2 with sigma of 0.04
 F61-F59
 2.2 with sigma of 0.04
 C33-C41 \\sim C33-C41A
 with sigma of 0.02
 C33-C83 \\sim C33-C83A
 with sigma of 0.02
 C33-C21 \\sim C33-C21A
 with sigma of 0.02
 F41-C41 \\sim F41A-C41A
 with sigma of 0.02
 F83-C41 \\sim F83A-C41A
 with sigma of 0.02
 F21-C83 \\sim F21A-C83A
 with sigma of 0.02
 F85-C21 \\sim F85A-C21A
 with sigma of 0.02
 F43-C21 \\sim F43A-C21A
 with sigma of 0.02
 F87-C83 \\sim F87A-C83A
 with sigma of 0.02
 F11-C41 \\sim F11A-C41A
 with sigma of 0.02
 F89-C83 \\sim F89A-C83A
 with sigma of 0.02
 C33-F41 \\sim C33-F41A
 with sigma of 0.04
 C33-F83 \\sim C33-F83A
 with sigma of 0.04
 C33-F21 \\sim C33-F21A
 with sigma of 0.04
 C33-F85 \\sim C33-F85A
 with sigma of 0.04
 C33-F43 \\sim C33-F43A
 with sigma of 0.04
 C33-F87 \\sim C33-F87A
 with sigma of 0.04
 C33-F11 \\sim C33-F11A
 with sigma of 0.04
 C33-F89 \\sim C33-F89A
 with sigma of 0.04
 F41-F83 \\sim F41A-F83A
 with sigma of 0.04
 F41-F11 \\sim F41A-F11A
 with sigma of 0.04
 F83-F11 \\sim F83A-F11A
 with sigma of 0.04
 F21-F87 \\sim F21A-F87A
 with sigma of 0.04
 F21-F89 \\sim F21A-F89A
 with sigma of 0.04
 F85-F43 \\sim F85A-F43A
 with sigma of 0.04
 F87-F89 \\sim F87A-F89A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C23 \\sim C50 \\sim O7 \\sim O5: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C33 \\sim O13 \\sim O2: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
F4 \\sim F14 \\sim F20 \\sim F22 \\sim F30 \\sim F36 \\sim F46 \\sim F52 \\sim
F64 \\sim C26 \\sim C44 \\sim C46 \\sim C54 \\sim F109 \\sim F55 \\sim F111
\\sim F7 \\sim F113 \\sim F57 \\sim F115 \\sim F29 \\sim F117 \\sim C93 \\sim
C47 \\sim C95 \\sim O12 \\sim O11: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
C84 \\sim C94 \\sim C55 \\sim C59 \\sim C61 \\sim C31 \\sim C67 \\sim C17 \\sim
C69 \\sim C35 \\sim C71 \\sim C9: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
C66 \\sim C78 \\sim C80 \\sim C86 \\sim C90 \\sim C53 \\sim C73 \\sim C37 \\sim
C75 \\sim C19 \\sim C77 \\sim C39: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
O3 \\sim O6: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
F93 \\sim F74 \\sim C43 \\sim C74 \\sim F44 \\sim F91 \\sim F108 \\sim F97:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C98 \\sim C87: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C85 \\sim C14 \\sim O9 \\sim O10: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F49 \\sim F118 \\sim C51 \\sim F99 \\sim F122 \\sim F88 \\sim F3 \\sim C11:
within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
C45 \\sim C29: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
F69 \\sim F35 \\sim F71 \\sim F73 \\sim F37 \\sim F75 \\sim F19 \\sim F77 \\sim
C79 \\sim C5 \\sim C81 \\sim F41 \\sim F83 \\sim F21 \\sim F85 \\sim F43 \\sim
F87 \\sim F11 \\sim F89 \\sim F45 \\sim C41 \\sim C83 \\sim C21 \\sim F41A
\\sim F83A \\sim F21A \\sim F85A \\sim F43A \\sim F87A \\sim F11A \\sim F89A
\\sim C41A \\sim C83A \\sim C21A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04 within 1.7A
3. Others
 Fixed Sof: F4(0.7872) F14(0.7872) F20(0.7872) F22(0.7872) F30(0.7872)
 F36(0.7872) O6(0.6668) F44(0.7633) F46(0.7872) F52(0.7872) F64(0.7872)
 O10(0.7633) F72(0.7633) F74(0.7633) F76(0.6668) F80(0.6668) F82(0.7633)
 O12(0.7872) F86(0.7633) O13(0.7865) F88(0.7633) F90(0.6668) O7(0.7754)
 F100(0.7754) F102(0.7754) F104(0.7754) F106(0.6668) F108(0.7633) F110(0.7754)
 F112(0.6668) C14(0.7633) F114(0.7754) F116(0.7754) F118(0.7633) F120(0.4291)
 F122(0.7633) F124(0.6668) C44(0.7872) F126(0.6668) C46(0.7872) F63(0.6179)
 C50(0.7754) C54(0.7872) C66(0.4291) H66(0.4291) F2(0.7754) C74(0.7633)
 C78(0.4291) C80(0.4291) H80(0.4291) C84(0.6179) F65(0.7754) C86(0.4291)
 H86(0.4291) F33(0.6179) C90(0.4291) H90(0.4291) C94(0.6179) H94(0.6179)
 C98(0.7633) C51(0.7633) F67(0.7754) C53(0.4291) C27(0.7754) C55(0.6179)
 H55(0.6179) C57(0.6668) C29(0.7754) C59(0.6179) H59(0.6179) C15(0.6668)
 C61(0.6179) C31(0.6179) H31(0.6179) F17(0.4291) C2(0.6668) C65(0.7754)
 F69(0.31) F35(0.31) F71(0.31) F73(0.31) F37(0.31) F75(0.31) F19(0.63)
 F77(0.31) C67(0.3821) H67(0.3821) C17(0.3821) H17(0.3821) C69(0.3821)
 H69(0.3821) C35(0.3821) C71(0.3821) C9(0.3821) H9(0.3821) F39(0.3821)
 F79(0.3821) F5(0.5709) C73(0.5709) C37(0.5709) F81(0.5709) C75(0.5709)
 H75(0.5709) C19(0.5709) H19(0.5709) C77(0.5709) H77(0.5709) C39(0.5709)
 H39(0.5709) C79(0.31) C5(0.31) C81(0.31) F41(0.37) F83(0.37) F21(0.37)
 F85(0.37) F43(0.37) F87(0.37) F11(0.37) F89(0.37) F45(0.37) C41(0.37)
 C83(0.37) C21(0.37) O2(0.2135) F91(0.2367) O9(0.2367) F23(0.2367) F93(0.2367)
 F47(0.2367) F95(0.2367) F3(0.2367) F97(0.2367) C85(0.2367) F49(0.2367)
 F99(0.2367) C43(0.2367) C87(0.2367) C11(0.2367) F25(0.2246) F101(0.2246)
 F51(0.2246) F103(0.2246) F13(0.2246) F105(0.2246) C89(0.2246) C45(0.2246)
 C91(0.2246) O5(0.2246) F53(0.2246) F107(0.2246) C23(0.2246) F27(0.2246)
 F109(0.2128) F55(0.2128) F111(0.2128) F7(0.2128) F113(0.2128) F57(0.2128)
 F115(0.2128) F29(0.2128) F117(0.2128) O11(0.2128) C93(0.2128) C47(0.2128)
 C95(0.2128) F59(0.3332) F119(0.3332) F15(0.3332) F121(0.3332) F61(0.3332)
 C3(0.3332) C97(0.3332) C49(0.3332) F123(0.3332) F125(0.3332) O3(0.3332)
 F41A(0.63) F83A(0.32) F21A(0.32) F85A(0.32) F43A(0.32) F87A(0.32) F11A(0.32)
 F89A(0.32) C41A(0.32) C83A(0.32) C21A(0.32)
 Fixed U11: C12(0.035528)
 Fixed U12: C12(0.007295)
 Fixed U13: C12(0.015978)
 Fixed U22: C12(0.06)
 Fixed U23: C12(0.004)
 Fixed U33: C12(0.047)
4.a Aromatic/amide H refined with riding coordinates:
 C28(H28), C66(H66), C76(H76), C80(H80), C86(H86), C90(H90), C94(H94),
 C55(H55), C7(H7), C59(H59), C31(H31), C63(H63), C67(H67), C17(H17), C69(H69),
 C9(H9), C75(H75), C19(H19), C77(H77), C39(H39)
4.b Idealised Me refined as rotating group:
 C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C56(H56A,H56B,H56C), C60(H60A,H60B,
 H60C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C68(H68A,H68B,H68C), C70(H70A,
 H70B,H70C), C72(H72A,H72B,H72C), C88(H88A,H88B,H88C)
;
_shelx_res_checksum              16330
_shelx_hkl_checksum              22809
_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 1.650
_oxdiff_exptl_absorpt_empirical_full_min 0.597