Homo- and heterobimetallic transition metal cluster derived from [Cp*Fe(η<sup>5</sup>-E<sub>5</sub>)] (E = P, As) - unprecedented structural motifs of the resulting polypnictogen ligands.
Dinauer, Sabrina B.; Szlosek, Robert; Piesch, Martin; Balázs, Gábor; Reichl, Stephan; Prock, Lukas; Riesinger, Christoph; Walter, Marc D.; Scheer, Manfred; Dalton transactions (Cambridge, England : 2003) 53 (2024) 10201–10207; doi:10.1039/d4dt01160k

data_7716174
_publ_section_title
;
 Homo- and heterobimetallic transition metal cluster derived from
 [Cp*Fe(&#x3b7;<sup>5</sup>-E<sub>5</sub>)] (E = P, As) - unprecedented
 structural motifs of the resulting polypnictogen ligands.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10201
_journal_page_last               10207
_journal_paper_doi               10.1039/d4dt01160k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C27 H44 Cr Fe P5'
_chemical_formula_sum            'C27 H44 Cr Fe P5'
_chemical_formula_weight         631.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-05-06
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-18 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.4680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.14730(10)
_cell_length_b                   13.60100(10)
_cell_length_c                   18.5936(2)
_cell_measurement_reflns_used    40575
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.7790
_cell_measurement_theta_min      3.2420
_cell_volume                     3010.62(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 42.92a 64-bit (release 29-05-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_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_temperature      123.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_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     -5.00  20.00   0.50    0.08    --    6.00 100.00-120.03   50
  2  \w     25.00  65.00   0.50    0.08    --   62.92 -95.00-150.00   80
  3  \w     33.00  62.00   0.50    0.08    --   62.92 -95.00 -90.00   58
  4  \w     40.00  68.00   0.50    0.36    --   75.56 -95.00-180.00   56
  5  \w     25.00  71.00   0.50    0.08    --   62.92 -95.00 -30.00   92
  6  \w     40.00  84.00   0.50    0.36    --   75.56 -95.00 -60.00   88
  7  \w     30.00  70.00   0.50    0.08    --   62.92 -95.00  30.00   80
  8  \w     39.00  81.00   0.50    0.08    --   73.03 -95.00 150.00   84
  9  \w     50.00  82.00   0.50    0.36    --   75.56 -95.00  90.00   64
 10  \w     38.00  84.00   0.50    0.36    --   75.56 -95.00  30.00   92
 11  \w     38.00  78.00   0.50    0.36    --   75.56 -95.00-150.00   80
 12  \w     18.00  43.00   0.50    0.08    --   22.00  90.00-127.17   50
 13  \w     74.00  99.00   0.50    0.08    --   70.00  76.00 -48.11   50
 14  \w     83.00 108.00   0.50    0.36    --   77.45  74.00 -72.13   50
 15  \w     60.00  85.00   0.50    0.08    --   54.00  73.00 -63.58   50
 16  \w     60.00  85.00   0.50    0.08    --   54.00  72.00 -74.01   50
 17  \w     68.00  95.00   0.50    0.08    --   62.00  72.00 -52.63   54
 18  \w     64.00  89.00   0.50    0.08    --   58.00  72.00 -52.82   50
 19  \w     60.00  85.00   0.50    0.08    --   54.00  73.00 -88.10   50
 20  \w     64.00  89.00   0.50    0.08    --   58.00  72.00 -97.68   50
 21  \w     68.00  93.00   0.50    0.08    --   62.00  72.00-106.29   50
 22  \w     65.00  90.00   0.50    0.08    --   58.00  71.00-133.63   50
 23  \w     75.00 100.00   0.50    0.08    --   70.00  74.00-148.37   50
 24  \w     65.00  90.00   0.50    0.08    --   58.00  71.00 -62.01   50
 25  \w     65.00  90.00   0.50    0.08    --   58.00  70.00 -89.90   50
 26  \w     69.00  94.00   0.50    0.08    --   62.00  70.00 -98.33   50
 27  \w     70.00  95.00   0.50    0.08    --   62.00  69.00 -87.06   50
 28  \w     70.00  95.00   0.50    0.08    --   62.00  69.00-128.21   50
 29  \w     65.00  90.00   0.50    0.08    --   58.00  70.00 -78.36   50
 30  \w     63.00  88.00   0.50    0.08    --   54.00  64.00-109.29   50
 31  \w     69.00  99.00   0.50    0.08    --   62.00  71.00 -20.24   60
 32  \w     98.00 123.00   0.50    0.36    --   77.45  43.00 -64.00   50
 33  \w     63.00  88.00   0.50    0.08    --   54.00  65.00 -13.08   50
 34  \w     63.00  88.00   0.50    0.08    --   54.00  71.00  27.02   50
 35  \w     65.00  93.00   0.50    0.08    --   73.03  25.00 175.00   56
 36  \w     56.00 110.00   0.50    0.08    --   62.92  25.00 175.00  108
 37  \w     82.00 108.00   0.50    0.36    --   75.56  25.00 175.00   52
 38  \w     43.00  95.00   0.50    0.36    --   75.56   0.00 150.00  104
 39  \w     32.00 108.00   0.50    0.08    --   62.92  15.00 120.00  152
 40  \w     26.00 100.00   0.50    0.08    --   62.92   0.00-120.00  148
 41  \w     41.00  66.00   0.50    0.08    --   38.00  77.00 -40.97   50
 42  \w     44.00  69.00   0.50    0.08    --   38.00  73.00 -74.86   50
 43  \w     43.00  68.00   0.50    0.08    --   38.00  75.00 -63.03   50
 44  \w     48.00  73.00   0.50    0.08    --   42.00  73.00 -32.21   50
 45  \w     32.00  57.00   0.50    0.08    --   26.00  73.00 -57.54   50
 46  \w     38.00  63.00   0.50    0.08    --   34.00  76.00-114.23   50
 47  \w     56.00  81.00   0.50    0.08    --   50.00  73.00-127.25   50
 48  \w     53.00  78.00   0.50    0.08    --   46.00  71.00-104.81   50
 49  \w     47.00  72.00   0.50    0.08    --   42.00  74.00 -95.68   50
 50  \w     53.00  78.00   0.50    0.08    --   46.00  71.00 -22.78   50
 51  \w     13.00  39.00   0.50    0.08    --    2.00  54.00-109.94   52
 52  \w    -90.00 -22.00   0.50    0.08    --  -63.82 125.00  60.00  136
 53  \w   -103.00 -55.00   0.50    0.36    --  -76.65 125.00-150.00   96
 54  \w    -79.00 -40.00   0.50    0.36    --  -76.65   0.00-150.00   78
 55  \w   -108.00 -82.00   0.50    0.36    --  -76.65   0.00-150.00   52
 56  \w   -106.00 -81.00   0.50    0.36    --  -78.07 -78.00 -44.24   50
 57  \w    -96.00 -70.00   0.50    0.08    --  -66.00 -75.00 -36.42   52
 58  \w   -101.00 -75.00   0.50    0.08    --  -70.00 -73.00 -56.48   52
 59  \w    -96.00 -70.00   0.50    0.08    --  -66.00 -75.00-118.55   52
 60  \w   -104.00 -79.00   0.50    0.08    --  -74.00 -75.00-139.51   50
 61  \w   -101.00 -76.00   0.50    0.08    --  -70.00 -74.00-135.41   50
 62  \w   -110.00 -79.00   0.50    0.08    --  -74.00 -73.00-103.94   62
 63  \w   -110.00 -85.00   0.50    0.36    --  -78.07 -73.00 -95.09   50
 64  \w   -100.00 -74.00   0.50    0.08    --  -66.00 -69.00 -79.90   52
 65  \w    -87.00 -61.00   0.50    0.08    --  -50.00 -69.00-132.15   52
 66  \w   -110.00 -80.00   0.50    0.08    --  -70.00 -64.00 -88.34   60
 67  \w   -107.00 -81.00   0.50    0.08    --  -70.00 -64.00 -95.23   52
 68  \w   -109.00 -83.00   0.50    0.08    --  -74.00 -64.00-101.16   52
 69  \w   -103.00 -78.00   0.50    0.08    --  -70.00 -65.00-110.08   50
 70  \w   -102.00 -76.00   0.50    0.08    --  -66.00 -61.00-153.24   52
 71  \w   -115.00 -89.00   0.50    0.08    --  -70.00 -46.00-156.45   52
 72  \w    -97.00 -71.00   0.50    0.08    --  -62.00 -62.00-103.36   52
 73  \w   -124.00 -91.00   0.50    0.36    --  -78.07 -39.00 -43.04   66
 74  \w   -120.00 -95.00   0.50    0.36    --  -76.65 -25.00  12.00   50
 75  \w   -117.00 -92.00   0.50    0.08    --  -73.46 -25.00  12.00   50
 76  \w   -108.00 -75.00   0.50    0.08    --  -63.82 -25.00  12.00   66
 77  \w   -109.00 -75.00   0.50    0.36    --  -76.65-125.00  90.00   68
 78  \w   -103.00 -78.00   0.50    0.36    --  -76.65-125.00 150.00   50
 79  \w   -117.00 -74.00   0.50    0.36    --  -76.65-125.00  60.00   86
 80  \w   -118.00 -91.00   0.50    0.36    --  -76.65-125.00 -60.00   54
 81  \w   -111.00 -86.00   0.50    0.36    --  -76.65-125.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            61137
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.178
_diffrn_reflns_theta_min         4.011
_exptl_absorpt_coefficient_mu    9.454
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.311
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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 red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.621
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0632P)^2^+1.5010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5673
_reflns_number_total             5942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01160k2.cif
_cod_data_source_block           sd509_f1_abs
_cod_depositor_comments
'Adding full bibliography for 7716174--7716180.cif.'
_cod_database_code               7716174
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.241
_shelx_estimated_absorpt_t_min   0.109
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C2(H2A,H2B,H2C),
 C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C5(H5A,H5B,H5C),
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), C3(H3A,H3B,H3C),
  C25(H25A,H25B,H25C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              18281
_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
;