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_7716176
_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 Fe3 P5'
_chemical_formula_sum            'C44 H73 Fe3 P5'
_chemical_formula_weight         924.42
_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                 106.6420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.23420(10)
_cell_length_b                   10.87860(10)
_cell_length_c                   22.55640(10)
_cell_measurement_reflns_used    22798
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.7810
_cell_measurement_theta_min      2.6500
_cell_volume                     4522.03(6)
_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 0.999
_diffrn_measured_fraction_theta_max 0.953
_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   -124.00 -36.00   0.50    0.50    --  -75.31 154.00-120.00  176
  2  \w   -102.00 -31.00   0.50    0.50    --  -75.31 121.00  80.00  142
  3  \w    -77.00 -52.00   0.50    0.50    --  -61.73 121.00  80.00   50
  4  \w     12.00  39.00   0.50    0.50    --   60.83 -30.00  60.00   54
  5  \w     13.00  40.00   0.50    0.50    --   60.83 -30.00  30.00   54
  6  \w     14.00  40.00   0.50    0.50    --   60.83 -30.00   0.00   52
  7  \w     12.00  37.00   0.50    0.50    --   60.83 -30.00 -30.00   50
  8  \w     13.00  40.00   0.50    0.50    --   60.83 -30.00 -60.00   54
  9  \w     48.00  75.00   0.50    0.50    --   81.79 -95.00-150.00   54
 10  \w     63.00  88.00   0.50    0.50    --   81.79-154.00-160.00   50
 11  \w     31.00  88.00   0.50    0.50    --   74.22-125.00 -30.00  114
 12  \w     49.00  74.00   0.50    0.50    --   81.79-121.00  -1.00   50
 13  \w     40.00  77.00   0.50    0.50    --   74.22 -95.00  30.00   74
 14  \w     49.00 110.00   0.50    0.50    --   81.79-125.00  60.00  122
 15  \w     57.00 111.00   0.50    0.50    --   81.79-125.00 120.00  108
 16  \w     17.00  66.00   0.50    0.50    --   60.83-121.00  -1.00   98
 17  \w     39.00  82.00   0.50    0.50    --   72.64 -95.00-180.00   86
 18  \w     74.00 122.00   0.50    0.50    --   72.64  30.00  30.00   96
 19  \w     75.00 124.00   0.50    0.50    --   74.22  30.00  90.00   98
 20  \w     86.00 128.00   0.50    0.50    --   81.79  30.00 120.00   84
 21  \w     92.00 117.00   0.50    0.50    --   81.79 125.00  30.00   50
 22  \w     90.00 115.00   0.50    0.50    --   81.79 154.00-120.00   50
 23  \w     62.00  87.00   0.50    0.50    --   72.64 154.00-120.00   50
 24  \w     83.00 110.00   0.50    0.50    --   81.79 125.00-180.00   54
 25  \w   -110.00 -75.00   0.50    0.50    --  -61.73 -30.00   0.00   70
 26  \w   -108.00 -83.00   0.50    0.50    --  -75.31-154.00-160.00   50
 27  \w    -83.00 -58.00   0.50    0.50    --  -73.07-154.00-160.00   50
 28  \w    -78.00 -53.00   0.50    0.50    --  -61.73-154.00-160.00   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  0.0229
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39583
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.254
_diffrn_reflns_theta_min         2.669
_exptl_absorpt_coefficient_mu    9.500
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.457
_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    1.358
_exptl_crystal_description       block
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         8917
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.7233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8333
_reflns_number_total             8917
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01160k2.cif
_cod_data_source_block           sd520_f2_abs
_cod_depositor_comments
'Adding full bibliography for 7716174--7716180.cif.'
_cod_database_code               7716176
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.648
_shelx_estimated_absorpt_t_min   0.371
_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), C6(H6), C12(H12), C26(H26)
2.b Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C11(H11A,H11B,H11C), C23(H23A,H23B,H23C), 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), 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              60975
_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
;