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_1575227
_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         'C54 Fe2 Mg O2 P12, 3[C4H8O]'
_chemical_formula_sum            'C66 H96 Fe2 Mg O5 P12'
_chemical_formula_weight         1477.07
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.73460(10)
_cell_length_b                   10.73460(10)
_cell_length_c                   60.8000(8)
_cell_measurement_reflns_used    10440
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      71.4480
_cell_measurement_theta_min      2.9080
_cell_volume                     7006.08(13)
_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      123.00(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.974
_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    -71.00 -45.00   0.50    4.00    --  -75.69 121.00  59.00   52
  2  \w   -119.00 -93.00   0.50    4.00    --  -75.69-121.00 -22.00   52
  3  \w     79.00 113.00   0.50    4.00    --   78.38-139.00  77.00   68
  4  \w     43.00  69.00   0.50    4.00    --   78.38-139.00  77.00   52
  5  \w     22.00  58.00   0.50    4.00    --   60.45 -95.00  60.00   72
  6  \w     11.00  36.00   0.50    4.00    --   60.45 -30.00  30.00   50
  7  \w   -106.00 -35.00   0.50    4.00    --  -61.39  -9.00  98.00  142
  8  \w   -118.00 -88.00   0.50    4.00    --  -75.69-125.00 -90.00   60
  9  \w    -88.00 -44.00   0.50    4.00    --  -80.00  96.00  42.52   88
 10  \w     60.00 128.00   0.50    4.00    --   82.00  13.00 122.65  136
 11  \w     37.00  63.00   0.50    4.00    --   82.00 -54.00   9.45   52
 12  \w     61.00 130.00   0.50    4.00    --   82.00  21.00 -54.55  138
 13  \w     37.00  62.00   0.50    4.00    --   82.00 -53.00 122.44   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  0.0496
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -75
_diffrn_reflns_number            30565
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.105
_diffrn_reflns_theta_min         4.182
_exptl_absorpt_coefficient_mu    6.377
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.755
_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            'clear intense brown'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       plate
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.418(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         6848
_refine_ls_number_restraints     297
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0556P)^2^+9.6899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.630
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.905
_reflns_number_gt                5884
_reflns_number_total             6848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04242a2.cif
_cod_data_source_block           maw459_3m_red1abs
_cod_depositor_comments
'Adding full bibliography for 1575224--1575230.cif.'
_cod_original_cell_volume        7006.08(16)
_cod_database_code               1575227
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C66 Fe2 H96 Mg1 O5 P12 '
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.697
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.582(9)
 0.418(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 O2-C1A = O2-C1D
 1.44 with sigma of 0.02
 C1A-C1B = C1C-C1D
 1.53 with sigma of 0.02
 C1B-C1C
 1.54 with sigma of 0.02
 O3-C1E = O3-C1H
 1.44 with sigma of 0.02
 C1E-C1F = C1G-C1H
 1.53 with sigma of 0.02
 C1F-C1G
 1.54 with sigma of 0.02
 O4-C1I = O4-C1L
 1.44 with sigma of 0.02
 C1I-C1J = C1K-C1L
 1.53 with sigma of 0.02
 C1J-C1K
 1.54 with sigma of 0.02
 O2-C1B = O2-C1C = C1A-C1C = C1B-C1D
 2.38 with sigma of 0.04
 O3-C1F = O3-C1G = C1E-C1G = C1F-C1H
 2.38 with sigma of 0.04
 O4-C1J = O4-C1K = C1I-C1K = C1J-C1L
 2.38 with sigma of 0.04
 C1A-C1B \\sim C1B-C1C \\sim C1C-C1D
 with sigma of 0.02
 O2-C1A \\sim O2-C1D
 with sigma of 0.02
 O2-C1B \\sim O2-C1C
 with sigma of 0.04
 C1B-C1D \\sim C1A-C1C
 with sigma of 0.04
 C1E-C1F \\sim C1F-C1G \\sim C1G-C1H
 with sigma of 0.02
 O3-C1E \\sim O3-C1H
 with sigma of 0.02
 O3-C1F \\sim O3-C1G
 with sigma of 0.04
 C1F-C1H \\sim C1E-C1G
 with sigma of 0.04
 C1I-C1J \\sim C1J-C1K \\sim C1K-C1L
 with sigma of 0.02
 O4-C1I \\sim O4-C1L
 with sigma of 0.02
 O4-C1J \\sim O4-C1K
 with sigma of 0.04
 C1J-C1L \\sim C1I-C1K
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
O2 \\sim C1A \\sim C1B \\sim C1C \\sim C1D: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O3 \\sim C1E \\sim C1F \\sim C1G \\sim C1H: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O2 \\sim C1A \\sim C1B \\sim C1C \\sim C1D \\sim O3 \\sim C1E \\sim C1F \\sim
C1G \\sim C1H: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
O4 \\sim C1I \\sim C1J \\sim C1K \\sim C1L: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
5. Rigid body (RIGU) restrains
 O2, C1A, C1B, C1C, C1D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3, C1E, C1F, C1G, C1H
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4, C1I, C1J, C1K, C1L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(O3)=Sof(C1E)=Sof(H1EA)=Sof(H1EB)=Sof(C1F)=Sof(H1FA)=Sof(H1FB)=Sof(C1G)=
 Sof(H1GA)=Sof(H1GB)=Sof(C1H)=Sof(H1HA)=Sof(H1HB)=1-FVAR(1)
 Sof(O2)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1C)=
 Sof(H1CA)=Sof(H1CB)=Sof(C1D)=Sof(H1DA)=Sof(H1DB)=FVAR(1)
 Fixed Sof: O4(0.5) C1I(0.5) H1IA(0.5) H1IB(0.5) C1J(0.5) H1JA(0.5) H1JB(0.5)
 C1K(0.5) H1KA(0.5) H1KB(0.5) C1L(0.5) H1LA(0.5) H1LB(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,H27B), C1A(H1AA,
 H1AB), C1B(H1BA,H1BB), C1C(H1CA,H1CB), C1D(H1DA,H1DB), C1E(H1EA,H1EB),
 C1F(H1FA,H1FB), C1G(H1GA,H1GB), C1H(H1HA,H1HB), C1I(H1IA,H1IB), C1J(H1JA,H1JB),
  C1K(H1KA,H1KB), C1L(H1LA,H1LB)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C13(H13), C15(H15), C16(H16),
 C17(H17), C19(H19)
7.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              96307
_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 1.244
_oxdiff_exptl_absorpt_empirical_full_min 0.812