A simple synthesis of group 2 anthracenides and their use as reducing agents for polypnictogen ligand complexes.
Adlbert, Lukas; Weber, Martin; Riesinger, Christoph; Seidl, Michael; Scheer, Manfred; Chemical science 16 (2025) 15446–15454; doi:10.1039/d5sc04242a

data_1575229
_publ_section_title
;
 A simple synthesis of group 2 anthracenides and their use as reducing
 agents for polypnictogen ligand complexes.
;
_journal_issue                   34
_journal_name_full               'Chemical science'
_journal_page_first              15446
_journal_page_last               15454
_journal_paper_doi               10.1039/d5sc04242a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C52 H94 Fe2 O8 P10 Sr2, 2(C4 H7 O)'
_chemical_formula_sum            'C60 H108 Fe2 O10 P10 Sr2'
_chemical_formula_weight         1586.10
_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             2025-01-13
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2025.01.10 svn.r16582094 for OlexSys, GUI svn.r7115)
;
_audit_update_record
;
2025-05-25 deposited with the CCDC.	2025-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.304(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.3561(3)
_cell_length_b                   15.5150(3)
_cell_length_c                   20.0866(5)
_cell_measurement_reflns_used    15844
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      25.3370
_cell_measurement_theta_min      2.7250
_cell_volume                     3747.36(15)
_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 1.5-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      140.00(10)
_diffrn_detector_area_resol_mean 10.5096
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.824
_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      7.00  32.00   0.50   60.50    --   -2.52-126.00 -60.00   50
  2  \w     17.00  42.00   0.50   60.50    --   -2.52-145.00 131.00   50
  3  \w      9.00  34.00   0.50   60.50    --    2.87-126.00 -60.00   50
  4  \w     20.00  46.00   0.50   60.50    --    2.87-145.00 131.00   52
  5  \w    -75.00 -31.00   0.50   60.50    --   -2.52 -57.00  90.00   88
  6  \w    -22.00  29.00   0.50   60.50    --    2.87  38.00  30.00  102
  7  \w    -21.00  77.00   0.50   60.50    --    2.87  38.00  90.00  196
  8  \w    -16.00  -8.50   0.50   60.50    --    2.87  38.00 -60.00   15
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.824
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            54161
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.824
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         25.986
_diffrn_reflns_theta_min         2.229
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.418
_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            'dark black'
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         12329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0621P)^2^+2.2627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9254
_reflns_number_total             12329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04242a2.cif
_cod_data_source_block           maw388_4agm_red1abs
_cod_depositor_comments
'Adding full bibliography for 1575224--1575230.cif.'
_cod_database_code               1575229
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C60H110Fe2O10P10Sr2
_shelx_estimated_absorpt_t_max   0.786
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H9BC)=Sof(H9BD)=Sof(H13C)=Sof(H13D)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=1-FVAR(1)
 Sof(H9AA)=Sof(H9AB)=Sof(H13A)=Sof(H13B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C29)=
 Sof(H29A)=Sof(H29B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C9(H9AA,H9AB), C9(H9BC,H9BD), C10(H10A,H10B),
 C13(H13A,H13B), C13(H13C,H13D), C14(H14A,H14B), C15(H15A,H15B), C17(H17A,H17B),
  C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,
 H16C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              87912
_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 39.736
_oxdiff_exptl_absorpt_empirical_full_min 0.322