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_7716180
_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 Ag Fe Ni2 P5, Al C36 F46 O3'
_chemical_formula_sum            'C80 H73 Ag Al F46 Fe Ni2 O3 P5'
_chemical_formula_weight         2419.35
_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             2023-10-17
_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                63.886(4)
_cell_angle_beta                 79.623(4)
_cell_angle_gamma                72.650(4)
_cell_formula_units_Z            2
_cell_length_a                   14.9140(6)
_cell_length_b                   19.2206(9)
_cell_length_c                   19.5632(9)
_cell_measurement_reflns_used    14969
_cell_measurement_temperature    122.98(10)
_cell_measurement_theta_max      73.8930
_cell_measurement_theta_min      3.5100
_cell_volume                     4798.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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      122.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.946
_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   -126.00 -37.00   1.00    5.00    --  -43.14 178.00 120.00   89
  2  \w     18.00 113.00   1.00    5.00    --   43.14  57.00 120.00   95
  3  \w    -27.00  69.00   1.00    5.00    --   43.14 -57.00 -30.00   96
  4  \w     80.00 178.00   1.00   20.00    --  104.50  30.00  30.00   98
  5  \w     30.00 127.00   1.00   20.00    --  104.50 -77.00-120.00   97
  6  \w     66.00 108.00   1.00   20.00    --  104.50-102.00  -9.00   42
  7  \w     65.00 178.00   1.00   20.00    --  104.50  15.00 -30.00  113
  8  \w     34.00  72.00   1.00   20.00    --  104.50 -45.00 150.00   38
  9  \w     35.00  91.00   1.00   20.00    --  104.50 -61.00   0.00   56
 10  \w     35.00  72.00   1.00   20.00    --  104.50 -45.00  30.00   37
 11  \w     45.00  70.00   1.00   20.00    --  104.50 -45.00   0.00   25
 12  \w     30.00  57.00   1.00   20.00    --  104.50-102.00  -9.00   27
 13  \w     35.00 121.00   1.00   20.00    --  104.50-137.00 170.22   86
 14  \w     22.00 107.00   1.00   20.00    --  104.50 -96.00 168.13   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0135388000
_diffrn_orient_matrix_UB_12      -0.0317872000
_diffrn_orient_matrix_UB_13      -0.0619567000
_diffrn_orient_matrix_UB_21      0.0409557000
_diffrn_orient_matrix_UB_22      0.0707668000
_diffrn_orient_matrix_UB_23      -0.0564758000
_diffrn_orient_matrix_UB_31      0.0994442000
_diffrn_orient_matrix_UB_32      -0.0497110000
_diffrn_orient_matrix_UB_33      0.0262344000
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31575
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.270
_diffrn_reflns_theta_min         2.643
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.352
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
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    1.674
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.138
_exptl_crystal_size_min          0.121
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1275
_refine_ls_number_reflns         18494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0349P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14896
_reflns_number_total             18494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01160k2.cif
_cod_data_source_block           ap_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7716174--7716180.cif.'
_cod_database_code               7716180
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C83H75AgAlF47FeNi2O3P5
_shelx_estimated_absorpt_t_max   0.564
_shelx_estimated_absorpt_t_min   0.399
_reflns_odcompleteness_completeness 99.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C3(H3), C5(H5), C20(H20)
1.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C33(H33A,H33B,H33C), C28(H28A,H28B,H28C), C15(H15A,H15B,H15C), C8(H8A,
 H8B,H8C), C34(H34A,H34B,H34C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C25(H25A,
 H25B,H25C), C41(H41A,H41B,H41C), C9(H9A,H9B,H9C), C42(H42A,H42B,H42C),
 C16(H16A,H16B,H16C), C32(H32A,H32B,H32C), C17(H17A,H17B,H17C), C29(H29A,H29B,
 H29C), C27(H27A,H27B,H27C), C43(H43A,H43B,H43C), C40(H40A,H40B,H40C), C44(H44A,
 H44B,H44C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              5332
_shelx_fab_checksum              38956
_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 1.722
_oxdiff_exptl_absorpt_empirical_full_min 0.754