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_7716177
_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 Fe3'
_chemical_formula_sum            'C44 H73 As5 Fe3'
_chemical_formula_weight         1144.17
_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                 106.2280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3773(2)
_cell_length_b                   10.87080(10)
_cell_length_c                   22.7856(2)
_cell_measurement_reflns_used    17143
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.3440
_cell_measurement_theta_min      2.6310
_cell_volume                     4608.48(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.948
_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     11.00  36.00   0.50    0.10    --   60.52 -30.00 150.00   50
  2  \w     16.00  42.00   0.50    0.10    --   60.52  -7.00  33.00   52
  3  \w     11.00  39.00   0.50    0.10    --   60.52 -30.00   0.00   56
  4  \w     12.00  39.00   0.50    0.10    --   60.52 -30.00 -90.00   54
  5  \w     54.00  79.00   0.50    0.10    --   74.57   7.00-151.00   50
  6  \w     62.00  95.00   0.50    0.10    --   60.52  30.00-120.00   66
  7  \w     36.00 105.00   0.50    0.10    --   60.52   7.00-151.00  138
  8  \w     40.00 107.00   0.50    0.10    --   74.02   7.00-151.00  134
  9  \w     96.00 122.00   0.50    0.10    --   74.57  30.00-120.00   52
 10  \w     62.00 110.00   0.50    0.10    --   60.52  30.00 120.00   96
 11  \w     37.00  85.00   0.50    0.10    --   74.57 -95.00  60.00   96
 12  \w     23.00  71.00   0.50    0.10    --   60.52 -95.00 -60.00   96
 13  \w     44.00  70.00   0.50    0.10    --   60.52 -95.00 -90.00   52
 14  \w     38.00  79.00   0.50    0.10    --   74.02 -95.00-150.00   82
 15  \w     27.00  52.00   0.50    0.10    --   60.52-125.00-150.00   50
 16  \w     64.00  89.00   0.50    0.10    --   60.52-125.00-150.00   50
 17  \w     53.00  79.00   0.50    0.10    --   74.02 -95.00 -90.00   52
 18  \w     36.00  76.00   0.50    0.10    --   74.57 -95.00 120.00   80
 19  \w    -74.00 -23.00   0.50    0.10    --  -61.43 125.00   0.00  102
 20  \w   -118.00 -38.00   0.50    0.10    --  -79.42 139.00 -81.11  160
 21  \w    -99.00 -35.00   0.50    0.10    --  -75.00 125.00 -90.00  128
 22  \w   -100.00 -74.00   0.50    0.10    --  -75.11 125.00-150.00   52
 23  \w    -59.00 -31.00   0.50    0.10    --  -75.11 125.00-150.00   56
 24  \w   -115.00 -40.00   0.50    0.10    --  -75.11  -7.00  33.00  150
 25  \w   -124.00 -97.00   0.50    0.10    --  -75.11 -30.00  30.00   54
 26  \w   -118.00 -73.00   0.50    0.10    --  -75.11-125.00  60.00   90
 27  \w    -52.00 -26.00   0.50    0.10    --  -61.43  -7.00  33.00   52
;
_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  0.0342
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40677
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.487
_diffrn_reflns_theta_min         2.653
_exptl_absorpt_coefficient_mu    11.670
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.360
_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    1.649
_exptl_crystal_description       plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0268
_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^)+(0.0294P)^2^+3.1728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0630
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7899
_reflns_number_total             8821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01160k2.cif
_cod_data_source_block           sd521_f1_abs
_cod_depositor_comments
'Adding full bibliography for 7716174--7716180.cif.'
_cod_database_code               7716177
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.593
_shelx_estimated_absorpt_t_min   0.215
_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:
 C4(H4), C18(H18), C20(H20), C34(H34)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C44(H44A,H44B,
 H44C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C27(H27A,
 H27B,H27C), C7(H7A,H7B,H7C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C2(H2A,
 H2B,H2C), C33(H33A,H33B,H33C), C17(H17A,H17B,H17C), C35(H35A,H35B,H35C),
 C9(H9A,H9B,H9C), C37(H37A,H37B,H37C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C),
  C5(H5A,H5B,H5C), C41(H41A,H41B,H41C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C)
;
_shelx_res_checksum              71136
_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
;