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_7131449
_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 Fe2 P5, B C24 F20, 0.5[CH2Cl2]'
_chemical_formula_sum            'C51.5 H45 B Cl F20 Fe2 P5'
_chemical_formula_weight         1356.68
_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                 104.7420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6478(3)
_cell_length_b                   19.8608(3)
_cell_length_c                   18.1588(2)
_cell_measurement_reflns_used    22791
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      71.5080
_cell_measurement_theta_min      2.2590
_cell_volume                     5457.58(15)
_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                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.991
_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     82.00 123.00   0.50    1.00    --   74.42  30.00 150.00   82
  2  \w     62.00 108.00   0.50    1.00    --   60.79  30.00  90.00   92
  3  \w     63.00 102.00   0.50    1.00    --   60.79  30.00 -30.00   78
  4  \w     89.00 124.00   0.50    1.00    --   74.37  30.00-120.00   70
  5  \w     78.00 120.00   0.50    1.00    --   74.37  30.00-150.00   84
  6  \w     72.00  97.00   0.50    1.00    --   74.37 137.00-148.00   50
  7  \w     19.00  90.00   0.50    1.00    --   60.79-125.00  30.00  142
  8  \w     46.00  71.00   0.50    1.00    --   74.37-133.00 -34.00   50
  9  \w     26.00  98.00   0.50    1.00    --   60.79-137.00 148.00  144
 10  \w     47.00  72.00   0.50    1.00    --   74.37-137.00 148.00   50
 11  \w     34.00  60.00   0.50    1.00    --   60.79-133.00 -34.00   52
 12  \w     34.00 102.00   0.50    1.00    --   74.37-125.00 -90.00  136
 13  \w     36.00  67.00   0.50    1.00    --   74.37 -95.00-180.00   62
 14  \w    -59.00 -22.00   0.50    1.00    --  -61.39 137.00-148.00   74
 15  \w    -95.00 -63.00   0.50    1.00    --  -61.39 137.00-148.00   64
 16  \w   -113.00 -59.00   0.50    1.00    --  -75.28 137.00-148.00  108
 17  \w   -104.00 -35.00   0.50    1.00    --  -75.28 125.00 -60.00  138
 18  \w    -96.00 -62.00   0.50    1.00    --  -75.28 133.00  33.00   68
 19  \w    -94.00 -69.00   0.50    1.00    --  -74.96 133.00  33.00   50
 20  \w    -95.00 -21.00   0.50    1.00    --  -61.39 133.00  33.00  148
 21  \w   -104.00 -32.00   0.50    1.00    --  -75.28 125.00   0.00  144
 22  \w   -111.00 -65.00   0.50    1.00    --  -61.39 -30.00   0.00   92
 23  \w   -113.00 -75.00   0.50    1.00    --  -75.28-125.00 -60.00   76
 24  \w   -118.00 -93.00   0.50    1.00    --  -75.28-133.00 -34.00   50
 25  \w   -118.00 -93.00   0.50    1.00    --  -74.96-133.00 -34.00   50
 26  \w   -119.00 -76.00   0.50    1.00    --  -74.96-125.00  30.00   86
 27  \w   -114.00 -66.00   0.50    1.00    --  -75.28-137.00 148.00   96
;
_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      -0.0000109000
_diffrn_orient_matrix_UB_12      -0.0776126000
_diffrn_orient_matrix_UB_13      0.0008182000
_diffrn_orient_matrix_UB_21      0.0743602000
_diffrn_orient_matrix_UB_22      0.0005689000
_diffrn_orient_matrix_UB_23      0.0741622000
_diffrn_orient_matrix_UB_31      -0.0694658000
_diffrn_orient_matrix_UB_32      0.0006779000
_diffrn_orient_matrix_UB_33      0.0467905000
_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  0.0479
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52174
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.122
_diffrn_reflns_theta_min         2.920
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.058
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.274
_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    1.651
_exptl_crystal_description       plate
_exptl_crystal_F_000             2732
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         10344
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0756P)^2^+1.4782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8525
_reflns_number_total             10344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00898c2.cif
_cod_data_source_block           cr1149
_cod_depositor_comments
'Adding full bibliography for 7131448--7131455.cif.'
_cod_original_formula_sum        'C51.50 H45 B Cl F20 Fe2 P5'
_cod_database_code               7131449
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C51H44BF20P5Fe2
_shelx_estimated_absorpt_t_max   0.677
_shelx_estimated_absorpt_t_min   0.234
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
C13 \\sim C47 \\sim C51 \\sim C23 \\sim C53 \\sim C25: within 1.7A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
2. Others
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(P2A)=Sof(P1A)=Sof(P5A)=Sof(P4A)=Sof(P3A)=1-FVAR(2)
 Sof(P3)=Sof(P4)=Sof(P2)=Sof(P1)=Sof(P5)=FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C50(H50)
3.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C35(H35A,H35B,H35C), C19(H19A,H19B,H19C), 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), C51(H51A,H51B,H51C),
  C13(H13A,H13B,H13C), C53(H53A,H53B,H53C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 84 electrons were 
found in a volume of 328\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.5[CH2Cl2] per Asymmetric Unit 
which account for 84 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38358
_shelx_hkl_checksum              46473
_shelx_fab_checksum              61133
_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 1.870
_oxdiff_exptl_absorpt_empirical_full_min 0.455