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_7131451
_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 Ni P5, B C24 F20, [+ solvents]0.5[CH2Cl2]'
_chemical_formula_sum            'C51 H44 B F20 Fe Ni P5'
_chemical_formula_weight         1317.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                 105.1610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8271(2)
_cell_length_b                   19.95370(10)
_cell_length_c                   17.9342(2)
_cell_measurement_reflns_used    32783
_cell_measurement_temperature    122.99(10)
_cell_measurement_theta_max      66.5800
_cell_measurement_theta_min      4.3140
_cell_volume                     5466.66(10)
_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    -44.00 -19.00   1.00    1.00    --  -43.23  25.00  38.00   25
  2  \w    -87.00 -61.00   1.00    1.00    --  -43.23 -25.00-125.00   26
  3  \w    -31.00  60.00   1.00    1.00    --   43.23 -25.00-125.00   91
  4  \w     44.00 114.00   1.00    1.00    --   43.23  25.00  38.00   70
  5  \w     84.00 109.00   1.00    3.00    --   86.50  25.00  38.00   25
  6  \w    -67.00 -42.00   1.00    3.00    --  -90.00  25.00  38.00   25
  7  \w   -142.00-106.00   1.00    3.00    --  -90.00 -25.00-125.00   36
  8  \w    -54.00 -27.00   1.00    1.00    --  -43.23  19.00 -90.00   27
  9  \w    -15.00  12.00   1.00    1.00    --  -43.23  19.00 -90.00   27
 10  \w      6.00  65.00   1.00    1.00    --   43.23-125.00-120.00   59
 11  \w   -156.00-130.00   1.00    3.00    --  -90.00-125.00  30.00   26
 12  \w   -161.00 -78.00   1.00    3.00    --  -90.00 -70.00 -51.97   83
 13  \w    -90.00 -64.00   1.00    3.00    --  -90.00 107.00 112.01   26
 14  \w   -157.00-131.00   1.00    3.00    --  -90.00 -94.00 -90.00   26
 15  \w   -155.00 -63.00   1.00    3.00    --  -90.00 -61.00  30.00   92
 16  \w    -86.00 -28.00   1.00    3.00    --  -90.00 125.00-180.00   58
 17  \w   -141.00-115.00   1.00    3.00    --  -90.00-107.00 157.27   26
 18  \w    -98.00 -64.00   1.00    3.00    --  -90.00  40.00  61.87   34
 19  \w    -80.00 -31.00   1.00    3.00    --  -90.00 125.00  30.00   49
 20  \w   -147.00-104.00   1.00    3.00    --  -90.00 -76.00 114.28   43
 21  \w   -130.00-104.00   1.00    3.00    --  -90.00 -46.00 147.37   26
 22  \w   -107.00 -81.00   1.00    3.00    --  -90.00  45.00 -90.00   26
 23  \w   -157.00-115.00   1.00    3.00    --  -90.00 -50.00 117.03   42
 24  \w    -56.00 -31.00   1.00    3.00    --  -90.00  45.00 -90.00   25
 25  \w    -63.00 -13.00   1.00    3.00    --  -90.00 107.00 112.01   50
 26  \w    -97.00 -35.00   1.00    3.00    --  -90.00 125.00  60.00   62
 27  \w   -134.00-104.00   1.00    3.00    --  -90.00 -77.00  60.00   30
 28  \w   -163.00-110.00   1.00    3.00    --  -90.00-125.00  60.00   53
 29  \w   -108.00 -76.00   1.00    3.00    --  -90.00 115.00 127.32   32
 30  \w    -67.00 -25.00   1.00    3.00    --  -90.00 115.00 127.32   42
 31  \w   -107.00 -81.00   1.00    3.00    --  -90.00 113.00 173.34   26
 32  \w   -160.00-124.00   1.00    3.00    --  -90.00 -69.00-171.91   36
 33  \w   -160.00 -98.00   1.00    3.00    --  -90.00-125.00   0.00   62
;
_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      -0.0460763000
_diffrn_orient_matrix_UB_12      -0.0182142000
_diffrn_orient_matrix_UB_13      0.0630372000
_diffrn_orient_matrix_UB_21      0.0841180000
_diffrn_orient_matrix_UB_22      0.0173023000
_diffrn_orient_matrix_UB_23      0.0628124000
_diffrn_orient_matrix_UB_31      -0.0313186000
_diffrn_orient_matrix_UB_32      0.0729771000
_diffrn_orient_matrix_UB_33      0.0009086000
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0411
_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       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52429
_diffrn_reflns_point_group_measured_fraction_full 0.803
_diffrn_reflns_point_group_measured_fraction_max 0.803
_diffrn_reflns_theta_full        66.813
_diffrn_reflns_theta_max         66.813
_diffrn_reflns_theta_min         3.644
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.886
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.308
_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 brown'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.219
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.488(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1449
_refine_ls_number_reflns         15560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0474P)^2^+4.1109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.565
_reflns_Friedel_fraction_full    0.598
_reflns_Friedel_fraction_max     0.598
_reflns_number_gt                15076
_reflns_number_total             15560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc00898c2.cif
_cod_data_source_block           as06_abs
_cod_depositor_comments
;
Adding full bibliography for 7131448--7131455.cif.

2024-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C102 H88 B2 F40 Fe2 Ni2 P10'
_cod_original_formula_weight         2634.16
_cod_original_formula_moiety
'2(C27 H44 Fe Ni P5), 2(B C24 F20), [+ solvents]1[CH2Cl2]'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5466.65(10)
_cod_database_code               7131451
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C103H88B2F40Fe2Ni2P10Cl2
_shelx_estimated_absorpt_t_max   0.414
_shelx_estimated_absorpt_t_min   0.329
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51216
 0.48784
2. Others
 Fixed X: Ni2(0.82961)
 Fixed Y: Ni2(0.20365)
 Fixed Z: Ni2(1.147282)
3.a Aromatic/amide H refined with riding coordinates:
 C68(H68), C80(H80), C77(H77), C39(H39)
3.b Idealised Me refined as rotating group:
 C60(H60A,H60B,H60C), C92(H92A,H92B,H92C), C51(H51A,H51B,H51C), C53(H53A,H53B,
 H53C), C7(H7A,H7B,H7C), C29(H29A,H29B,H29C), C61(H61A,H61B,H61C), C65(H65A,
 H65B,H65C), C33(H33A,H33B,H33C), C69(H69A,H69B,H69C), C35(H35A,H35B,H35C),
 C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C37(H37A,H37B,H37C), C11(H11A,H11B,
 H11C), C89(H89A,H89B,H89C), C45(H45A,H45B,H45C), C91(H91A,H91B,H91C), C23(H23A,
 H23B,H23C), C93(H93A,H93B,H93C), C47(H47A,H47B,H47C), C95(H95A,H95B,H95C),
 C3(H3A,H3B,H3C), C97(H97A,H97B,H97C), C49(H49A,H49B,H49C), C99(H99A,H99B,H99C),
  C25(H25A,H25B,H25C), C101(H10A,H10B,H10C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 100 electrons were 
found in a volume of 404\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
[+ solvents]1[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              46118
_shelx_hkl_checksum              88499
_shelx_fab_checksum              69192
_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 2.245
_oxdiff_exptl_absorpt_empirical_full_min 0.670