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_7131454
_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 Fe3 P10, 0.92(C H2 Cl2), 2(B C24 F20)'
_chemical_formula_sum            'C69 H32 B2 Cl2 F40 Fe3 P10'
_chemical_formula_weight         2190.71
_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                 91.7850(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4743(2)
_cell_length_b                   20.2790(2)
_cell_length_c                   20.0413(2)
_cell_measurement_reflns_used    35356
_cell_measurement_temperature    123.02(10)
_cell_measurement_theta_max      71.9870
_cell_measurement_theta_min      3.0580
_cell_volume                     7910.86(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      123.02(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 0.996
_diffrn_measured_fraction_theta_max 0.961
_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   -103.00 -38.00   0.50    1.50    --  -67.57 -12.00 111.00  130
  2  \w     90.00 115.00   0.50    1.50    --   72.89  12.00 -76.00   50
  3  \w     54.00  85.00   0.50    1.50    --   72.89  12.00 -76.00   62
  4  \w     38.00  86.00   0.50    1.50    --   66.97   0.00 -90.00   96
  5  \w     50.00  75.00   0.50    1.50    --   66.97  12.00 -76.00   50
  6  \w     45.00  92.00   0.50    1.50    --   66.97-125.00   0.00   94
  7  \w     80.00 109.00   0.50    1.50    --   66.97  12.00 -76.00   58
  8  \w     35.00  61.00   0.50    1.50    --   66.97-125.00  30.00   52
  9  \w     26.00  90.00   0.50    1.50    --   66.97-125.00  90.00  128
 10  \w   -104.00 -52.00   0.50    1.50    --  -67.57 -15.00 -90.00  104
 11  \w   -110.00 -43.00   0.50    1.50    --  -67.57 -15.00  30.00  134
 12  \w     64.00  91.00   0.50    1.50    --   72.89-125.00 -30.00   54
 13  \w     62.00  88.00   0.50    1.50    --   72.89-125.00-180.00   52
 14  \w     56.00  99.00   0.50    1.50    --   72.89-125.00 150.00   86
 15  \w     37.00  64.00   0.50    1.50    --   72.89-125.00-120.00   54
 16  \w     67.00 114.00   0.50    1.50    --   72.89  15.00  30.00   94
 17  \w     40.00  69.00   0.50    1.50    --   72.89   0.00-120.00   58
 18  \w     31.00  62.00   0.50    1.50    --   72.89-125.00 -30.00   62
 19  \w     41.00  68.00   0.50    1.50    --   72.89-125.00   0.00   54
 20  \w     73.00 100.00   0.50    1.50    --   72.89   0.00-120.00   54
 21  \w     66.00  94.00   0.50    1.50    --   72.89-125.00-120.00   56
 22  \w   -101.00 -40.00   0.50    1.50    --  -73.25 132.00 -79.49  122
 23  \w    -94.00 -41.00   0.50    1.50    --  -73.25 116.00  14.69  106
 24  \w    -72.00 -37.00   0.50    1.50    --  -73.25 145.00  10.25   70
 25  \w   -103.00 -78.00   0.50    1.50    --  -73.25 -83.00-152.20   50
 26  \w   -111.00 -85.00   0.50    1.50    --  -73.25 145.00  10.25   52
 27  \w     51.00 119.00   0.50    1.50    --   76.00-153.00 109.76  136
 28  \w     50.00 112.00   0.50    1.50    --   77.25  16.00  99.15  124
 29  \w     38.00  97.00   0.50    1.50    --   77.25-113.00  33.23  118
 30  \w     60.00  91.00   0.50    1.50    --   77.25-110.00 -72.12   62
 31  \w     59.00 121.00   0.50    1.50    --   77.25  19.00 149.74  124
;
_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      0.0474504000
_diffrn_orient_matrix_UB_12      -0.0114150000
_diffrn_orient_matrix_UB_13      -0.0589825000
_diffrn_orient_matrix_UB_21      0.0624863000
_diffrn_orient_matrix_UB_22      -0.0035963000
_diffrn_orient_matrix_UB_23      0.0489466000
_diffrn_orient_matrix_UB_31      -0.0102085000
_diffrn_orient_matrix_UB_32      -0.0750198000
_diffrn_orient_matrix_UB_33      0.0066361000
_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  0.0379
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            85089
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.152
_diffrn_reflns_theta_min         3.101
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.166
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.302
_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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_description       plate
_exptl_crystal_F_000             4312
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         15714
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0850P)^2^+10.0196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12105
_reflns_number_total             15714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00898c2.cif
_cod_data_source_block           cr965
_cod_depositor_comments
'Adding full bibliography for 7131448--7131455.cif.'
_cod_database_code               7131454
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C68H30B2F40P10Fe3
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.267
_olex2_refinement_description
;
1. Restrained distances
 P10-P8 \\sim P10A-P8A
 with sigma of 0.04
 P5-P3 \\sim P5A-P3A
 with sigma of 0.04
 P1-P3 \\sim P1A-P3A
 with sigma of 0.04
 P5-P1 \\sim P5A-P1A
 with sigma of 0.02
 P5-P4 \\sim P5A-P4A
 with sigma of 0.02
 P1-P2 \\sim P1A-P2A
 with sigma of 0.02
 P6-P9 \\sim P6A-P9A
 with sigma of 0.04
 P6-P10 \\sim P6A-P10A
 with sigma of 0.02
 P6-P7 \\sim P6A-P7A
 with sigma of 0.02
 P7-P9 \\sim P7A-P9A
 with sigma of 0.04
 P10-P9 \\sim P10A-P9A
 with sigma of 0.02
 P7-P8 \\sim P7A-P8A
 with sigma of 0.02
 P4-P3 \\sim P4A-P3A
 with sigma of 0.02
 P1-P4 \\sim P1A-P4A
 with sigma of 0.04
 P2-P3 \\sim P2A-P3A
 with sigma of 0.02
 P6-P8 \\sim P6A-P8A
 with sigma of 0.04
 P8-P9 \\sim P8A-P9A
 with sigma of 0.02
 P10-P7 \\sim P10A-P7A
 with sigma of 0.04
 P4-P2 \\sim P4A-P2A
 with sigma of 0.04
 Fe1-P5 \\sim Fe1-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-P2 \\sim Fe1-P2A
 with sigma of 0.04
 Fe1-P3 \\sim Fe1-P3A
 with sigma of 0.04
 Fe3-P5 \\sim Fe3-P5A
 with sigma of 0.04
 Fe3-P1 \\sim Fe3-P1A
 with sigma of 0.04
 Fe3-P6 \\sim Fe3-P6A
 with sigma of 0.04
 Fe3-P10 \\sim Fe3-P10A
 with sigma of 0.04
 Fe3-P7 \\sim Fe3-P7A
 with sigma of 0.04
 Fe3-P4 \\sim Fe3-P4A
 with sigma of 0.04
 Fe3-P2 \\sim Fe3-P2A
 with sigma of 0.04
 Fe3-P8 \\sim Fe3-P8A
 with sigma of 0.04
 Fe3-P3 \\sim Fe3-P3A
 with sigma of 0.04
 Fe3-P9 \\sim Fe3-P9A
 with sigma of 0.04
 Fe2-P6 \\sim Fe2-P6A
 with sigma of 0.04
 Fe2-P10 \\sim Fe2-P10A
 with sigma of 0.04
 Fe2-P7 \\sim Fe2-P7A
 with sigma of 0.04
 Fe2-P8 \\sim Fe2-P8A
 with sigma of 0.04
 Fe2-P9 \\sim Fe2-P9A
 with sigma of 0.04
 P5-P2 \\sim P5A-P2A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
P6 \\sim P10 \\sim P7 \\sim P8 \\sim P9 \\sim P6A \\sim P10A \\sim P7A \\sim
P8A \\sim P9A: within 2.2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2.2A
P5 \\sim P1 \\sim P4 \\sim P2 \\sim P3 \\sim P5A \\sim P1A \\sim P4A \\sim P2A
\\sim P3A: within 2.2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2.2A
3. Others
 Sof(P5A)=Sof(P1A)=Sof(P4A)=Sof(P2A)=Sof(P3A)=Sof(P6A)=Sof(P10A)=Sof(P7A)=
 Sof(P8A)=Sof(P9A)=1-FVAR(1)
 Sof(P5)=Sof(P1)=Sof(P6)=Sof(P10)=Sof(P7)=Sof(P4)=Sof(P2)=Sof(P8)=Sof(P3)=
 Sof(P9)=FVAR(1)
 Fixed Sof: Cl2(0.92) Cl1(0.92) C17(0.92) H17A(0.92) H17B(0.92)
4.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B)
4.b Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C), C2(H2A,H2B,H2C), C65(H65A,
 H65B,H65C), C33(H33A,H33B,H33C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              47897
_shelx_hkl_checksum              28659
_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 1.255
_oxdiff_exptl_absorpt_empirical_full_min 0.801