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_7131452
_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 Co Fe2 P10, Al C16 F36 O4, 0.5(C6 H4 F2)'
_chemical_formula_sum            'C39 H32 Al Co F37 Fe2 O4 P10'
_chemical_formula_weight         1774.95
_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             2022-11-17
_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                 96.7550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.87740(10)
_cell_length_b                   28.6587(3)
_cell_length_c                   20.0246(2)
_cell_measurement_reflns_used    23485
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      66.8090
_cell_measurement_theta_min      3.7630
_cell_volume                     6198.98(11)
_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      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -65.00 -34.00   1.00    2.00    --  -43.68  89.00-111.00   31
  2  \w     24.00  59.00   1.00    2.00    --   43.68 -89.00 133.00   35
  3  \w    101.00 126.00   1.00    8.00    --   86.50  89.00-111.00   25
  4  \w     42.00  67.00   1.00    8.00    --   86.50 -89.00 133.00   25
  5  \w    -95.00 -56.00   1.00    8.00    --  -90.00  89.00-111.00   39
  6  \w   -138.00-113.00   1.00    8.00    --  -90.00 -89.00 133.00   25
  7  \w    -95.00 -68.00   1.00    2.00    --  -43.68 -57.00-150.00   27
  8  \w      8.00  86.00   1.00    2.00    --   43.68-125.00  90.00   78
  9  \w     21.00 109.00   1.00    2.00    --   43.68  57.00-120.00   88
 10  \w   -163.00-115.00   1.00    8.00    --  -90.00 -77.00-180.00   48
 11  \w   -163.00-104.00   1.00    8.00    --  -90.00 -77.00 150.00   59
 12  \w   -103.00 -69.00   1.00    8.00    --  -90.00 125.00  90.00   34
 13  \w   -163.00-121.00   1.00    8.00    --  -90.00-125.00-120.00   42
 14  \w   -163.00-126.00   1.00    8.00    --  -90.00-125.00  60.00   37
 15  \w   -147.00 -99.00   1.00    8.00    --  -90.00-125.00  90.00   48
 16  \w   -156.00-108.00   1.00    8.00    --  -90.00 -94.00  30.00   48
 17  \w   -101.00 -64.00   1.00    8.00    --  -90.00  77.00-120.00   37
 18  \w    -46.00 -19.00   1.00    8.00    --  -90.00  77.00-120.00   27
 19  \w   -104.00 -45.00   1.00    8.00    --  -90.00  45.00 120.00   59
 20  \w   -168.00-143.00   1.00    8.00    --  -90.00 -15.00   0.00   25
 21  \w   -114.00 -87.00   1.00    8.00    --  -90.00 -15.00   0.00   27
 22  \w    -54.00 -25.00   1.00    8.00    --  -90.00  74.00 -91.55   29
 23  \w   -117.00 -27.00   1.00    8.00    --  -90.00  77.00 -60.00   90
 24  \w   -140.00-115.00   1.00    8.00    --  -90.00 -15.00   0.00   25
 25  \w   -123.00 -67.00   1.00    8.00    --  -90.00 -30.00-180.00   56
 26  \w   -107.00 -17.00   1.00    8.00    --  -90.00  30.00-150.00   90
 27  \w   -130.00 -97.00   1.00    8.00    --  -90.00 -30.00 -60.00   33
 28  \w   -164.00-117.00   1.00    8.00    --  -90.00 -94.00-120.00   47
 29  \w   -158.00-133.00   1.00    8.00    --  -90.00   0.00-180.00   25
 30  \w    -67.00 -42.00   1.00    8.00    --  -90.00   0.00-180.00   25
 31  \w    -87.00 -60.00   1.00    8.00    --  -90.00 125.00-120.00   27
 32  \w   -105.00 -64.00   1.00    8.00    --  -90.00 125.00  60.00   41
 33  \w    -54.00 -29.00   1.00    8.00    --  -90.00 125.00  90.00   25
 34  \w    -51.00 -26.00   1.00    8.00    --  -90.00  45.00-120.00   25
 35  \w    -68.00 -43.00   1.00    8.00    --  -90.00  61.00-120.00   25
 36  \w    -82.00 -55.00   1.00    8.00    --  -90.00  96.00-171.66   27
 37  \w   -157.00-130.00   1.00    8.00    --  -90.00 -77.00  60.00   27
 38  \w   -155.00-116.00   1.00    8.00    --  -90.00 -94.00 -90.00   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0220139000
_diffrn_orient_matrix_UB_12      -0.0477785000
_diffrn_orient_matrix_UB_13      -0.0346390000
_diffrn_orient_matrix_UB_21      0.1404746000
_diffrn_orient_matrix_UB_22      -0.0093582000
_diffrn_orient_matrix_UB_23      0.0094814000
_diffrn_orient_matrix_UB_31      -0.0115581000
_diffrn_orient_matrix_UB_32      -0.0227978000
_diffrn_orient_matrix_UB_33      0.0686159000
_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  0.0698
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            66406
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.984
_diffrn_reflns_theta_max         66.984
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.782
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.118
_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            'dark green'
_exptl_crystal_density_diffrn    1.902
_exptl_crystal_description       plate
_exptl_crystal_F_000             3492
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         10977
_refine_ls_number_restraints     1392
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0585P)^2^+10.3923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9296
_reflns_number_total             10977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00898c2.cif
_cod_data_source_block           cr1107
_cod_depositor_comments
'Adding full bibliography for 7131448--7131455.cif.'
_cod_database_code               7131452
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C39H32O4F37AlP10Fe2Co
_shelx_estimated_absorpt_t_max   0.473
_shelx_estimated_absorpt_t_min   0.164
_olex2_refinement_description
;
1. Restrained distances
 F3-C47 = F25-C47
 1.33 with sigma of 0.02
 F9-C9
 1.3 with sigma of 0.02
 F37-C37
 1.3 with sigma of 0.02
 F25-F3
 2.2 with sigma of 0.04
 F1-F25
 2.2 with sigma of 0.04
 F1-F3
 2.2 with sigma of 0.04
 C43-C11
 2.55 with sigma of 0.04
 C44-C16 \\sim C3-C23 \\sim C49-C23 \\sim C48-C16 \\sim C32-C16 \\sim C47-C23
 with sigma of 0.02
 O3-C16 \\sim O5-C23
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 1.7A
C34A \\sim C34: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C9 \\sim C37 \\sim C19 \\sim C39 \\sim C5 \\sim C41 \\sim F9 \\sim F37: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C43 \\sim C36 \\sim C45 \\sim C46: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C47 \\sim C32: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C3 \\sim C44 \\sim F53 \\sim F46: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F6 \\sim F39: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F40 \\sim F51: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C23 \\sim C16: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F40 \\sim F44 \\sim F29 \\sim C48 \\sim F51 \\sim F13 \\sim F27 \\sim C49:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F3 \\sim F20 \\sim F36 \\sim F25: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F12 \\sim F32 \\sim C42 \\sim F5 \\sim F11 \\sim C11 \\sim F6 \\sim F39: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F35A \\sim F35: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C15A \\sim C15: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(C47) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C12) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
3. Others
 Sof(F19)=Sof(F39)=Sof(F5)=Sof(F41)=Sof(F21)=Sof(F43)=Sof(O2)=Sof(F11)=
 Sof(F45)=Sof(F23)=Sof(C21)=Sof(C43)=Sof(C11)=Sof(C45)=1-FVAR(1)
 Sof(F4)=Sof(F6)=Sof(F12)=Sof(F22)=Sof(F24)=Sof(F26)=Sof(O6)=Sof(F32)=Sof(F38)=
 Sof(F42)=Sof(C12)=Sof(C36)=Sof(C42)=Sof(C46)=FVAR(1)
 Sof(F47)=Sof(F3)=Sof(F49)=Sof(F25)=Sof(F51)=Sof(F13)=Sof(F53)=Sof(F27)=
 Sof(C23)=Sof(C47)=Sof(C3)=Sof(C49)=Sof(O5)=1-FVAR(2)
 Sof(F10)=Sof(F20)=Sof(F30)=Sof(F36)=Sof(F40)=Sof(F44)=Sof(O3)=Sof(F46)=
 Sof(F29)=Sof(C16)=Sof(C32)=Sof(C44)=Sof(C48)=FVAR(2)
 Sof(F18A)=Sof(F28A)=Sof(F34A)=Sof(F50A)=Sof(F54A)=Sof(F2A)=Sof(F33A)=
 Sof(F17A)=Sof(F35A)=Sof(C34A)=Sof(C25A)=Sof(C15A)=Sof(C31A)=1-FVAR(3)
 Sof(F18)=Sof(F28)=Sof(F34)=Sof(F50)=Sof(F54)=Sof(F2)=Sof(F33)=Sof(F17)=
 Sof(F35)=Sof(C34)=Sof(C25)=Sof(C15)=Sof(C31)=FVAR(3)
 Fixed Sof: C9(0.5) C37(0.5) C19(0.5) H19(0.5) C39(0.5) H39(0.5) C5(0.5)
 H5(0.5) C41(0.5) H41(0.5) F9(0.5) F37(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C39(H39), C5(H5), C41(H41)
4.b Fitted hexagon refined as free rotating group:
 C9(C37,C19,C39,C5,C41)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C40(H40A,H40B,H40C), C29(H29A,H29B,H29C), C2(H2A,H2B,H2C), C33(H33A,
 H33B,H33C), C17(H17A,H17B,H17C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              38221
_shelx_hkl_checksum              68354
_olex2_date_sample_data_collection 2022-08-10
_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 1.931
_oxdiff_exptl_absorpt_empirical_full_min 0.675