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_7131450
_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         'C27 H44 Fe Mn P5, Al C16 F36 O4'
_chemical_formula_sum            'C43 H44 Al F36 Fe Mn O4 P5'
_chemical_formula_weight         1601.40
_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                 93.7580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.95740(10)
_cell_length_b                   21.6035(2)
_cell_length_c                   23.2630(2)
_cell_measurement_reflns_used    35210
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      66.5920
_cell_measurement_theta_min      4.2010
_cell_volume                     5996.42(9)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -43.00 -18.00   1.00    2.00    --  -43.23  84.00-123.00   25
  2  \w    -32.00  21.00   1.00    2.00    --   43.23 -84.00 116.00   53
  3  \w     39.00  65.00   1.00    2.00    --   43.23 -84.00 116.00   26
  4  \w     94.00 119.00   1.00    8.00    --   86.50  84.00-123.00   25
  5  \w    -67.00 -41.00   1.00    8.00    --  -90.00  84.00-123.00   26
  6  \w   -124.00 -99.00   1.00    8.00    --  -90.00  84.00-123.00   25
  7  \w    -95.00 -29.00   1.00    2.00    --  -43.23 125.00 -30.00   66
  8  \w    -91.00 -42.00   1.00    2.00    --  -43.23 125.00  30.00   49
  9  \w     20.00 115.00   1.00    2.00    --   43.23  37.00-120.00   95
 10  \w     40.00  65.00   1.00    8.00    --   86.50 -84.00 116.00   25
 11  \w   -152.00-107.00   1.00    8.00    --  -90.00 -77.00 150.00   45
 12  \w   -119.00 -76.00   1.00    8.00    --  -90.00 -59.00 122.32   43
 13  \w   -164.00-127.00   1.00    8.00    --  -90.00 -77.00-120.00   37
 14  \w   -162.00-105.00   1.00    8.00    --  -90.00 -77.00  90.00   57
 15  \w   -156.00 -66.00   1.00    8.00    --  -90.00 -55.00-167.54   90
 16  \w   -154.00-129.00   1.00    8.00    --  -90.00-125.00-120.00   25
 17  \w   -118.00 -63.00   1.00    8.00    --  -90.00 -64.00-176.17   55
 18  \w   -158.00-128.00   1.00    8.00    --  -90.00 -59.00 122.32   30
 19  \w   -127.00-101.00   1.00    8.00    --  -90.00  -7.00-174.77   26
 20  \w   -145.00-113.00   1.00    8.00    --  -90.00 -45.00-150.00   32
 21  \w   -155.00-129.00   1.00    8.00    --  -90.00 -64.00 157.33   26
 22  \w   -142.00-117.00   1.00    8.00    --  -90.00-125.00  60.00   25
 23  \w   -164.00-118.00   1.00    8.00    --  -90.00-125.00 -90.00   46
 24  \w   -104.00 -79.00   1.00    8.00    --  -90.00 -64.00 157.33   25
 25  \w   -110.00 -84.00   1.00    8.00    --  -90.00 -70.00 158.14   26
 26  \w   -112.00 -77.00   1.00    8.00    --  -90.00  53.00  96.91   35
 27  \w    -69.00 -43.00   1.00    8.00    --  -90.00  53.00  96.91   26
 28  \w   -117.00 -66.00   1.00    8.00    --  -90.00  61.00-120.00   51
 29  \w   -146.00-116.00   1.00    8.00    --  -90.00 -63.00 -68.14   30
 30  \w   -102.00 -64.00   1.00    8.00    --  -90.00 -63.00 -68.14   38
 31  \w   -156.00-113.00   1.00    8.00    --  -90.00 -59.00  17.22   43
 32  \w    -98.00 -66.00   1.00    8.00    --  -90.00 -45.00-150.00   32
 33  \w    -91.00 -28.00   1.00    8.00    --  -90.00 125.00  60.00   63
 34  \w    -78.00 -52.00   1.00    8.00    --  -90.00 125.00 -60.00   26
 35  \w   -100.00 -74.00   1.00    8.00    --  -90.00 125.00  30.00   26
 36  \w   -105.00 -43.00   1.00    8.00    --  -90.00  96.00-160.17   62
 37  \w   -112.00 -27.00   1.00    8.00    --  -90.00 125.00   0.00   85
 38  \w   -140.00-102.00   1.00    8.00    --  -90.00 -84.00 116.00   38
;
_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      -0.0606806000
_diffrn_orient_matrix_UB_12      0.0629486000
_diffrn_orient_matrix_UB_13      -0.0014016000
_diffrn_orient_matrix_UB_21      -0.0108743000
_diffrn_orient_matrix_UB_22      -0.0039690000
_diffrn_orient_matrix_UB_23      0.0655292000
_diffrn_orient_matrix_UB_31      0.1133750000
_diffrn_orient_matrix_UB_32      0.0333120000
_diffrn_orient_matrix_UB_33      0.0105185000
_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  0.0488
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63995
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.753
_diffrn_reflns_theta_max         66.753
_diffrn_reflns_theta_min         3.705
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.488
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.350
_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    1.774
_exptl_crystal_description       block
_exptl_crystal_F_000             3188
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.163
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1179
_refine_ls_number_reflns         10585
_refine_ls_number_restraints     1041
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0540P)^2^+5.3926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0961
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10027
_reflns_number_total             10585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00898c2.cif
_cod_data_source_block           as18
_cod_depositor_comments
'Adding full bibliography for 7131448--7131455.cif.'
_cod_database_code               7131450
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C43H44AlF36FeMnO4P5
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.284
_olex2_refinement_description
;
1. Restrained distances
 F11-C45 = F21-C45 = F43-C45
 1.33 with sigma of 0.02
 F37-C43 = F9-C43 = F41-C43
 1.33 with sigma of 0.02
 F39-C11 = F5-C11 = F19-C11
 1.33 with sigma of 0.02
 C51-C25 = C39-C25 = C25-C13
 1.53 with sigma of 0.02
 F29-C39A = F31-C39A = F59-C39A
 1.33 with sigma of 0.02
 C39A-C25
 1.53 with sigma of 0.02
 F9-F37
 2.2 with sigma of 0.04
 F19-F5
 2.2 with sigma of 0.04
 F41-F9
 2.2 with sigma of 0.04
 F11-F21
 2.2 with sigma of 0.04
 F39-F19
 2.2 with sigma of 0.04
 F21-F43
 2.2 with sigma of 0.04
 F5-F39
 2.2 with sigma of 0.04
 F43-F11
 2.2 with sigma of 0.04
 F37-F41
 2.2 with sigma of 0.04
 F31-F59
 2.2 with sigma of 0.04
 F59-F29
 2.2 with sigma of 0.04
 F29-F31
 2.2 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
F20 \\sim F56 \\sim F60 \\sim F62 \\sim C46 \\sim F63 \\sim F2 \\sim F33 \\sim
F17 \\sim F35 \\sim C5 \\sim C41 \\sim C21 \\sim F9 \\sim F37 \\sim F19 \\sim
F39 \\sim F5 \\sim F41 \\sim F21 \\sim F43 \\sim C43 \\sim C11 \\sim C45 \\sim
F11: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within
1.7A
F4 \\sim F12 \\sim F18 \\sim F24 \\sim F26 \\sim F30 \\sim F44 \\sim F46 \\sim
F48 \\sim F54 \\sim C27 \\sim C2 \\sim C33 \\sim C37 \\sim F23 \\sim F47 \\sim
F3 \\sim F49 \\sim F25 \\sim F51 \\sim F13 \\sim F53 \\sim C23 \\sim C47 \\sim
C3 \\sim C49: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
F60 \\sim F62 \\sim C41 \\sim F9 \\sim F37 \\sim F41 \\sim C43 \\sim F2: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F1 \\sim F8 \\sim F10 \\sim F24 \\sim F28 \\sim F36 \\sim F42 \\sim F50 \\sim
F58 \\sim C42 \\sim C7 \\sim C9 \\sim C39 \\sim F27 \\sim F55 \\sim F7 \\sim
F57 \\sim F29 \\sim F59 \\sim F15 \\sim F61 \\sim F31 \\sim C25 \\sim C51 \\sim
C13 \\sim O3 \\sim O2: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C39A \\sim C39: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
3. Others
 Sof(F9)=Sof(F37)=Sof(F19)=Sof(F39)=Sof(F5)=Sof(F41)=Sof(F21)=Sof(F43)=
 Sof(C43)=Sof(C11)=Sof(C45)=Sof(F11)=1-FVAR(1)
 Sof(F20)=Sof(F56)=Sof(F60)=Sof(F62)=Sof(F63)=Sof(F2)=Sof(F33)=Sof(F17)=
 Sof(F35)=Sof(C5)=Sof(C41)=Sof(C21)=FVAR(1)
 Sof(F23)=Sof(F47)=Sof(F3)=Sof(F49)=Sof(F25)=Sof(F51)=Sof(F13)=Sof(F53)=
 Sof(C23)=Sof(C47)=Sof(C3)=Sof(C49)=1-FVAR(2)
 Sof(F12)=Sof(F18)=Sof(F26)=Sof(F30)=Sof(F44)=Sof(F46)=Sof(F48)=Sof(F54)=
 Sof(C27)=Sof(C2)=Sof(C33)=Sof(C37)=FVAR(2)
 Sof(O2)=Sof(F27)=Sof(F55)=Sof(F7)=Sof(F57)=Sof(F29)=Sof(F59)=Sof(F15)=
 Sof(F61)=Sof(F31)=Sof(C25)=Sof(C51)=Sof(C13)=Sof(C39A)=1-FVAR(3)
 Sof(F1)=Sof(F8)=Sof(F10)=Sof(O3)=Sof(F24)=Sof(F28)=Sof(F36)=Sof(F42)=Sof(F50)=
 Sof(F58)=Sof(C42)=Sof(C7)=Sof(C9)=Sof(C39)=FVAR(3)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C10(H10)
4.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C32(H32A,H32B,
 H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C44(H44A,
 H44B,H44C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C29(H29A,H29B,H29C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              12866
_shelx_hkl_checksum              4994
_olex2_date_sample_data_collection 2022-05-10
_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 1.488
_oxdiff_exptl_absorpt_empirical_full_min 0.787