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_7131448
_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 Cr Fe P5, B C24 F20, 0.5(C6 H4 F2)'
_chemical_formula_sum            'C54 H46 B Cr F21 Fe P5'
_chemical_formula_weight         1367.42
_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                 104.2570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7984(2)
_cell_length_b                   19.8256(2)
_cell_length_c                   18.1573(2)
_cell_measurement_reflns_used    27730
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      66.5400
_cell_measurement_theta_min      3.9640
_cell_volume                     5511.94(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      122.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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    -88.00 -63.00   1.00    4.00    --  -43.23 128.00 -49.00   25
  2  \w    -95.00 -70.00   1.00    4.00    --  -43.23 141.00 122.00   25
  3  \w     68.00 114.00   1.00    4.00    --   43.23 141.00 122.00   46
  4  \w     56.00  84.00   1.00    4.00    --   43.23-141.00  65.00   28
  5  \w     24.00  49.00   1.00    4.00    --   43.23-128.00-123.00   25
  6  \w     32.00  58.00   1.00   16.00    --   86.50-141.00  65.00   26
  7  \w     92.00 117.00   1.00   16.00    --   86.50 128.00 -49.00   25
  8  \w   -104.00 -79.00   1.00   16.00    --  -90.00 141.00 122.00   25
  9  \w   -148.00-122.00   1.00   16.00    --  -90.00-141.00  65.00   26
 10  \w    -70.00 -44.00   1.00   16.00    --  -90.00 128.00 -49.00   26
 11  \w    -71.00 -38.00   1.00    4.00    --  -43.23 125.00 120.00   33
 12  \w    -59.00 -19.00   1.00    4.00    --  -43.23 -57.00  60.00   40
 13  \w   -103.00 -78.00   1.00    4.00    --  -43.23 -57.00  60.00   25
 14  \w     19.00 113.00   1.00    4.00    --   43.23  57.00 150.00   94
 15  \w   -110.00 -59.00   1.00   16.00    --  -90.00 125.00 150.00   51
 16  \w   -117.00 -91.00   1.00   16.00    --  -90.00 -30.00  30.00   26
 17  \w   -135.00-109.00   1.00   16.00    --  -90.00-125.00  30.00   26
 18  \w   -160.00-131.00   1.00   16.00    --  -90.00 -66.00 105.54   29
 19  \w   -161.00-136.00   1.00   16.00    --  -90.00-125.00  30.00   25
 20  \w   -111.00 -80.00   1.00   16.00    --  -90.00 -66.00 105.54   31
 21  \w   -105.00 -79.00   1.00   16.00    --  -90.00 -50.00  20.40   26
 22  \w   -160.00-105.00   1.00   16.00    --  -90.00 -61.00 -60.00   55
 23  \w   -112.00 -71.00   1.00   16.00    --  -90.00 124.00  -9.48   41
 24  \w    -54.00 -29.00   1.00   16.00    --  -90.00 124.00  -9.48   25
 25  \w   -109.00 -83.00   1.00   16.00    --  -90.00  77.00 -60.00   26
 26  \w    -96.00 -36.00   1.00   16.00    --  -90.00 125.00 120.00   60
 27  \w   -126.00 -97.00   1.00   16.00    --  -90.00-125.00-180.00   29
 28  \w    -57.00 -31.00   1.00   16.00    --  -90.00  77.00 -60.00   26
 29  \w   -157.00 -73.00   1.00   16.00    --  -90.00 -61.00  15.07   84
 30  \w   -123.00 -83.00   1.00   16.00    --  -90.00  81.00  86.78   40
 31  \w    -64.00 -38.00   1.00   16.00    --  -90.00  81.00  86.78   26
 32  \w   -114.00 -62.00   1.00   16.00    --  -90.00 -69.00-131.35   52
 33  \w   -163.00-137.00   1.00   16.00    --  -90.00-125.00-180.00   26
 34  \w   -115.00 -66.00   1.00   16.00    --  -90.00 -53.00 -58.36   49
 35  \w    -70.00 -45.00   1.00   16.00    --  -90.00 125.00  60.00   25
 36  \w   -144.00-114.00   1.00   16.00    --  -90.00 -77.00-120.00   30
 37  \w   -116.00 -91.00   1.00   16.00    --  -90.00  61.00 150.00   25
 38  \w    -97.00 -31.00   1.00   16.00    --  -90.00 125.00-120.00   66
 39  \w   -109.00 -83.00   1.00   16.00    --  -90.00 125.00  30.00   26
 40  \w   -102.00 -67.00   1.00   16.00    --  -90.00 125.00  90.00   35
 41  \w   -122.00 -85.00   1.00   16.00    --  -90.00 137.00-154.05   37
 42  \w   -159.00-113.00   1.00   16.00    --  -90.00 -69.00-151.18   46
 43  \w   -142.00-104.00   1.00   16.00    --  -90.00 -77.00 150.00   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      0.0569048000
_diffrn_orient_matrix_UB_12      -0.0050392000
_diffrn_orient_matrix_UB_13      -0.0575703000
_diffrn_orient_matrix_UB_21      0.0005320000
_diffrn_orient_matrix_UB_22      0.0774840000
_diffrn_orient_matrix_UB_23      -0.0062359000
_diffrn_orient_matrix_UB_31      0.0829872000
_diffrn_orient_matrix_UB_32      0.0029457000
_diffrn_orient_matrix_UB_33      0.0656362000
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            57435
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        66.730
_diffrn_reflns_theta_max         66.730
_diffrn_reflns_theta_min         3.647
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.102
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.156
_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 brown'
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       plate
_exptl_crystal_F_000             2756
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         9708
_refine_ls_number_restraints     200
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0693P)^2^+2.4250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8818
_reflns_number_total             9708
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00898c2.cif
_cod_data_source_block           as14
_cod_depositor_comments
'Adding full bibliography for 7131448--7131455.cif.'
_cod_database_code               7131448
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C54H46BF21P5CrFe
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.205
_olex2_refinement_description
;
1. Restrained distances
 P1-P2 \\sim P1A-P2A
 with sigma of 0.04
 Cr1-P5 \\sim Cr1-P5A
 with sigma of 0.02
 Cr1-P2 \\sim Cr1-P2A
 with sigma of 0.02
 P4-P2 \\sim P4A-P2A
 with sigma of 0.04
 P1-P4 \\sim P1A-P4A
 with sigma of 0.02
 P5-P3 \\sim P5A-P3A
 with sigma of 0.04
 P1-P5 \\sim P1A-P5A
 with sigma of 0.02
 P4-P3 \\sim P4A-P3A
 with sigma of 0.02
 Cr1-P4 \\sim Cr1-P4A
 with sigma of 0.04
 Cr1-P3 \\sim Cr1-P3A
 with sigma of 0.04
 P1-P3 \\sim P1A-P3A
 with sigma of 0.04
 P3-P2 \\sim P3A-P2A
 with sigma of 0.02
 P4-P5 \\sim P4A-P5A
 with sigma of 0.04
 Fe1-P1 \\sim Fe1-P1A
 with sigma of 0.04
 Fe1-P4 \\sim Fe1-P4A
 with sigma of 0.04
 Fe1-P5 \\sim Fe1-P5A
 with sigma of 0.04
 Fe1-P3 \\sim Fe1-P3A
 with sigma of 0.04
 Fe1-P2 \\sim Fe1-P2A
 with sigma of 0.04
 P5-P2 \\sim P5A-P2A
 with sigma of 0.02
 Cr1-P1 \\sim Cr1-P1A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
C45 \\sim C45A: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 1.7A
C7 \\sim C55 \\sim C27 \\sim C53 \\sim C13 \\sim C51 \\sim F5 \\sim F21: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
P1 \\sim P4 \\sim P5 \\sim P3 \\sim P2 \\sim P5A \\sim P2A \\sim P3A \\sim P4A
\\sim P1A: within 2.5A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2.5A
3. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C45A)=Sof(H45D)=Sof(H45E)=Sof(H45F)=Sof(C49A)=Sof(H49D)=Sof(H49E)=
 Sof(H49F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=1-FVAR(2)
 Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(H45C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=FVAR(2)
 Sof(P5A)=Sof(P2A)=Sof(P3A)=Sof(P4A)=Sof(P1A)=1-FVAR(3)
 Sof(P1)=Sof(P4)=Sof(P5)=Sof(P3)=Sof(P2)=FVAR(3)
 Fixed Sof: C51(0.5) C13(0.5) C53(0.5) H53(0.5) C27(0.5) H27(0.5) C55(0.5)
 H55(0.5) C7(0.5) H7(0.5) F5(0.5) F21(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C32(H32), C53(H53), C27(H27), C55(H55), C7(H7)
4.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C5(H5A,H5B,
 H5C), C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C), C11(H11A,
 H11B,H11C), C45(H45A,H45B,H45C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C),
 C3(H3A,H3B,H3C), C49(H49A,H49B,H49C), C25(H25A,H25B,H25C), C3A(H3AA,H3AB,H3AC),
  C23A(H23D,H23E,H23F), C25A(H25D,H25E,H25F), C45A(H45D,H45E,H45F), C49A(H49D,
 H49E,H49F), C47A(H47D,H47E,H47F)
;
_shelx_res_checksum              66974
_shelx_hkl_checksum              32199
_olex2_date_sample_data_collection 2022-04-21
_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 1.747
_oxdiff_exptl_absorpt_empirical_full_min 0.707