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_7716175
_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 Fe Mn P5'
_chemical_formula_sum            'C27 H44 Fe Mn P5'
_chemical_formula_weight         634.26
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-15
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-18 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.14780(10)
_cell_length_b                   13.55300(10)
_cell_length_c                   18.5913(2)
_cell_measurement_reflns_used    28267
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.0310
_cell_measurement_theta_min      3.9580
_cell_volume                     2997.80(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.83a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-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      100.00(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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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     71.00 122.00   0.50    0.10    --   79.50  22.00-148.86  102
  2  \w     66.00  94.00   0.50    0.10    --   78.00  23.00-106.93   56
  3  \w     90.00 116.00   0.50    0.10    --   79.50  21.00 -88.74   52
  4  \w     65.00 104.00   0.50    0.10    --   79.50  22.00  43.22   78
  5  \w     92.00 124.00   0.50    0.10    --   79.50  44.00  49.08   64
  6  \w     91.00 117.00   0.50    0.10    --   79.50  16.00 151.38   52
  7  \w     72.00 120.00   0.50    0.10    --   78.00  23.00 174.60   96
  8  \w     52.00  78.00   0.50    0.10    --   79.50  16.00 151.38   52
  9  \w     49.00  90.00   0.50    0.10    --   79.50   4.00 176.36   82
 10  \w     38.00  91.00   0.50    0.10    --   62.52  15.00 150.00  106
 11  \w     46.00 104.00   0.50    0.10    --   79.50   4.00  36.56  116
 12  \w     52.00  88.00   0.50    0.10    --   62.52   0.00 -90.00   72
 13  \w     53.00  81.00   0.50    0.10    --   79.50 -87.00  77.70   56
 14  \w     82.00 110.00   0.50    0.10    --   79.50-128.00 121.45   56
 15  \w     46.00  72.00   0.50    0.10    --   79.50-128.00 121.45   52
 16  \w     63.00 109.00   0.50    0.10    --   79.50-126.00  77.29   92
 17  \w     46.00  72.00   0.50    0.10    --   79.50-126.00 -46.89   52
 18  \w     45.00 121.00   0.50    0.10    --   79.50-166.00 -57.56  152
 19  \w     84.00 109.00   0.50    0.10    --   79.50-126.00 -46.89   50
 20  \w     84.00 111.00   0.50    0.10    --   79.50-130.00-162.07   54
 21  \w     52.00  78.00   0.50    0.10    --   75.28-125.00-150.00   52
 22  \w     36.00  62.00   0.50    0.10    --   79.50-130.00-162.07   52
 23  \w     41.00  90.00   0.50    0.10    --   75.28-125.00  30.00   98
 24  \w     35.00  84.00   0.50    0.10    --   75.56-125.00  60.00   98
 25  \w     33.00  58.00   0.50    0.10    --   75.28-125.00  90.00   50
 26  \w     42.00  68.00   0.50    0.10    --   79.50-124.00  79.54   52
 27  \w     73.00  98.00   0.50    0.10    --   75.28-125.00 150.00   50
 28  \w     40.00  81.00   0.50    0.10    --   79.50-123.00  -1.19   82
 29  \w     83.00 108.00   0.50    0.10    --   79.50-124.00  -2.51   50
 30  \w     54.00  95.00   0.50    0.10    --   79.50-120.00 -17.47   82
 31  \w     36.00  98.00   0.50    0.10    --   79.50-124.00 -79.53  124
 32  \w     59.00  85.00   0.50    0.10    --   79.50-116.00 -95.77   52
 33  \w     29.00  54.00   0.50    0.10    --   62.52 -95.00-180.00   50
 34  \w     25.00  70.00   0.50    0.10    --   62.52 -95.00-120.00   90
 35  \w     39.00  68.00   0.50    0.10    --   75.56 -95.00 -90.00   58
 36  \w     69.00  94.00   0.50    0.10    --   79.50-104.00 -26.82   50
 37  \w     40.00  70.00   0.50    0.10    --   75.56 -95.00  30.00   60
 38  \w     33.00  69.00   0.50    0.10    --   62.52 -95.00  90.00   72
 39  \w     57.00  83.00   0.50    0.10    --   79.50-114.00 163.50   52
 40  \w     37.00  69.00   0.50    0.10    --   75.28 -95.00 120.00   64
 41  \w     41.00  66.00   0.50    0.10    --   75.56 -95.00  60.00   50
 42  \w     39.00  65.00   0.50    0.10    --   75.56 -95.00-150.00   52
 43  \w     42.00 110.00   0.50    0.10    --   79.50  -1.00 -51.68  136
 44  \w     38.00  63.00   0.50    0.10    --   79.50 -54.00 -51.05   50
 45  \w     44.00 100.00   0.50    0.10    --   79.50  -2.00-111.68  112
 46  \w     89.00 115.00   0.50    0.10    --   79.50 157.00-172.04   52
 47  \w    -78.00 -51.00   0.50    0.10    --  -75.50 131.00 -63.53   54
 48  \w    -99.00 -68.00   0.50    0.10    --  -70.22 125.00   0.00   62
 49  \w    -69.00 -26.00   0.50    0.10    --  -70.22 125.00 -60.00   86
 50  \w    -51.00 -26.00   0.50    0.10    --  -70.22 125.00   0.00   50
 51  \w    -67.00 -39.00   0.50    0.10    --  -75.50 123.00   7.51   56
 52  \w   -103.00 -74.00   0.50    0.10    --  -75.50 123.00   7.51   58
 53  \w    -66.00 -41.00   0.50    0.10    --  -75.50  64.00  72.62   50
 54  \w    -69.00 -33.00   0.50    0.10    --  -70.22   0.00-120.00   72
 55  \w   -108.00 -38.00   0.50    0.10    --  -70.22   0.00-180.00  140
 56  \w   -103.00 -78.00   0.50    0.10    --  -75.50 -80.00  14.50   50
 57  \w   -107.00 -81.00   0.50    0.10    --  -75.50 -74.00  21.22   52
 58  \w   -111.00 -85.00   0.50    0.10    --  -75.50 -66.00  22.56   52
 59  \w    -98.00 -73.00   0.50    0.10    --  -70.00 -79.00  47.90   50
 60  \w   -105.00 -79.00   0.50    0.10    --  -75.50 -76.00  41.70   52
 61  \w   -116.00 -90.00   0.50    0.10    --  -75.50 -46.00  96.91   52
 62  \w    -97.00 -39.00   0.50    0.10    --  -70.22 -15.00 120.00  116
 63  \w    -98.00 -42.00   0.50    0.10    --  -63.96 -15.00-120.00  112
 64  \w   -119.00 -94.00   0.50    0.10    --  -75.50-129.00-172.52   50
 65  \w   -109.00 -84.00   0.50    0.10    --  -75.50 -83.00  17.65   50
 66  \w   -108.00 -82.00   0.50    0.10    --  -75.50 -83.00  28.24   52
 67  \w   -105.00 -80.00   0.50    0.10    --  -75.50 -83.00  40.83   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_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0604129000
_diffrn_orient_matrix_UB_12      -0.0933034000
_diffrn_orient_matrix_UB_13      -0.0352415000
_diffrn_orient_matrix_UB_21      0.0065967000
_diffrn_orient_matrix_UB_22      -0.0450502000
_diffrn_orient_matrix_UB_23      0.0768348000
_diffrn_orient_matrix_UB_31      -0.1143577000
_diffrn_orient_matrix_UB_32      0.0467101000
_diffrn_orient_matrix_UB_33      0.0036870000
_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  0.0573
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59246
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.220
_diffrn_reflns_theta_min         4.007
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.935
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.156
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.83a (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            'brownish green'
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         6140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0595P)^2^+1.2635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5702
_reflns_number_total             6140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01160k2.cif
_cod_data_source_block           abs_gaus_erroroff
_cod_depositor_comments
'Adding full bibliography for 7716174--7716180.cif.'
_cod_database_code               7716175
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         (C17H29C10H15FeP5Mn)2
_shelx_estimated_absorpt_t_max   0.382
_shelx_estimated_absorpt_t_min   0.182
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C008(H008), C00A(H00A)
1.b Idealised Me refined as rotating group:
 C00I(H00B,H00C,H00D), C00K(H00E,H00F,H00G), C00L(H00H,H00I,H00J), C00N(H00K,
 H00L,H00M), C00O(H00N,H00O,H00P), C00P(H00Q,H00R,H00S), C00Q(H00T,H00U,H00V),
 C00S(H00W,H00X,H00Y), C00T(H00Z,H,HA), C00U(H00,HB,HC), C00V(H1,HD,HE),
 C00W(H2,HF,HG), C00X(H3,HH,HI), C00Y(H4,HJ,HK)
;
_shelx_res_checksum              38996
_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 2.774
_oxdiff_exptl_absorpt_empirical_full_min 0.591