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_7716178
_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         'C44 H73 As5 Fe Ni2, 0.2[C2H3N]'
_chemical_formula_sum            'C44 H73 As5 Fe Ni2'
_chemical_formula_weight         1149.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                72.5910(10)
_cell_angle_beta                 70.5950(10)
_cell_angle_gamma                64.918(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4331(2)
_cell_length_b                   12.5276(2)
_cell_length_c                   17.9814(3)
_cell_measurement_reflns_used    26138
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      72.8450
_cell_measurement_theta_min      3.9540
_cell_volume                     2351.07(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection
'CrysAlisPro system (CCD 43.91a 64-bit (release 29-09-2023))'
_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 0.986
_diffrn_measured_fraction_theta_max 0.954
_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     37.00  68.00   0.50    0.05    --   73.03   0.00-180.00   62
  2  \w     82.00 108.00   0.50    0.05    --   73.03   0.00-180.00   52
  3  \w     58.00  84.00   0.50    0.05    --   62.92   0.00 -30.00   52
  4  \w     27.00  53.00   0.50    0.05    --   62.92   0.00 -30.00   52
  5  \w     38.00  95.00   0.50    0.05    --   75.56   0.00 120.00  114
  6  \w     40.00  66.00   0.50    0.05    --   75.56 -95.00 -30.00   52
  7  \w     67.00 103.00   0.50    0.05    --   73.03-130.00  38.00   72
  8  \w     30.00  62.00   0.50    0.05    --   62.92-130.00  38.00   64
  9  \w     44.00  69.00   0.50    0.05    --   75.56-130.00  38.00   50
 10  \w     81.00 106.00   0.50    0.05    --   75.56-130.00  38.00   50
 11  \w     76.00 102.00   0.50    0.05    --   75.56-125.00 -60.00   52
 12  \w     47.00  72.00   0.50    0.05    --   73.03-141.00-134.00   50
 13  \w     51.00  77.00   0.50    0.05    --   62.92-141.00-134.00   52
 14  \w     74.00 101.00   0.50    0.05    --   75.56-125.00 -90.00   54
 15  \w     43.00  69.00   0.50    0.05    --   75.56-125.00 -60.00   52
 16  \w     36.00  61.00   0.50    0.05    --   75.56-125.00 -90.00   50
 17  \w     32.00  71.00   0.50    0.05    --   62.92 -95.00 -90.00   78
 18  \w     35.00 102.00   0.50    0.05    --   75.56-125.00 -30.00  134
 19  \w     44.00  79.00   0.50    0.05    --   73.03 -95.00  30.00   70
 20  \w     51.00 102.00   0.50    0.05    --   75.56-125.00  90.00  102
 21  \w     38.00  70.00   0.50    0.05    --   75.56 -95.00 150.00   64
 22  \w     25.00  71.00   0.50    0.05    --   62.92 -95.00  30.00   92
 23  \w     26.00  58.00   0.50    0.05    --   62.92 -95.00-120.00   64
 24  \w     88.00 113.00   0.50    0.05    --   75.56 141.00 -76.00   50
 25  \w    -98.00 -41.00   0.50    0.05    --  -63.82 141.00 -76.00  114
 26  \w    -99.00 -74.00   0.50    0.05    --  -76.65 141.00 -76.00   50
 27  \w    -54.00 -25.00   0.50    0.05    --  -63.82 125.00  60.00   58
 28  \w   -100.00 -33.00   0.50    0.05    --  -73.46 125.00  30.00  134
 29  \w    -85.00 -59.00   0.50    0.05    --  -63.82 125.00  60.00   52
 30  \w   -102.00 -76.00   0.50    0.05    --  -76.65 125.00  60.00   52
 31  \w   -106.00 -80.00   0.50    0.05    --  -76.65 130.00 110.00   52
 32  \w    -99.00 -71.00   0.50    0.05    --  -73.46 130.00 110.00   56
 33  \w   -102.00 -57.00   0.50    0.05    --  -76.65 125.00 150.00   90
 34  \w    -94.00 -35.00   0.50    0.05    --  -63.82 130.00 110.00  118
 35  \w    -62.00 -35.00   0.50    0.05    --  -76.65 125.00  60.00   54
 36  \w   -107.00 -32.00   0.50    0.05    --  -63.82 -15.00-150.00  150
 37  \w   -101.00 -45.00   0.50    0.05    --  -76.65 -15.00 -30.00  112
 38  \w   -107.00 -39.00   0.50    0.05    --  -63.82 -15.00  90.00  136
 39  \w   -100.00 -44.00   0.50    0.05    --  -63.82 -15.00 150.00  112
 40  \w    -92.00 -67.00   0.50    0.05    --  -73.46-141.00-134.00   50
 41  \w   -117.00 -91.00   0.50    0.05    --  -76.65-125.00-180.00   52
 42  \w   -115.00 -90.00   0.50    0.05    --  -76.65-141.00-134.00   50
 43  \w   -116.00 -74.00   0.50    0.05    --  -76.65-125.00 -30.00   84
 44  \w   -113.00 -70.00   0.50    0.05    --  -73.46-130.00  38.00   86
 45  \w   -112.00 -87.00   0.50    0.05    --  -76.65-130.00  38.00   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  0.0228
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33114
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.011
_diffrn_reflns_theta_min         3.965
_exptl_absorpt_coefficient_mu    7.484
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.085
_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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         8990
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0260
_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^)+(0.0334P)^2^+1.8530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8889
_reflns_number_total             8990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01160k2.cif
_cod_data_source_block           sd530_f3_abs
_cod_depositor_comments
'Adding full bibliography for 7716174--7716180.cif.'
_cod_database_code               7716178
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.400
_shelx_estimated_absorpt_t_min   0.137
_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. Uiso/Uaniso restraints and constraints
As1A \\sim As1: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(As1) \\sim Ueq, Uanis(As1A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
3. Others
 Sof(As1A)=1-FVAR(1)
 Sof(As1)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C28(H28), C34(H34)
4.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C), C42(H42A,H42B,
 H42C), C44(H44A,H44B,H44C), C3(H3A,H3B,H3C), C25(H25A,H25B,H25C), C13(H13A,
 H13B,H13C), C27(H27A,H27B,H27C), C7(H7A,H7B,H7C), C29(H29A,H29B,H29C),
 C15(H15A,H15B,H15C), C31(H31A,H31B,H31C), C2(H2A,H2B,H2C), C33(H33A,H33B,H33C),
  C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C37(H37A,H37B,H37C), C19(H19A,H19B,
 H19C), C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C43(H43A,
 H43B,H43C)
;
_shelx_res_checksum              41458
_platon_squeeze_void_probe_radius 1.20
_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
;