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_1575225
_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         '2(C52 H69 Fe Mg N2 P6), C5 H12'
_chemical_formula_sum            'C109 H150 Fe2 Mg2 N4 P12'
_chemical_formula_weight         2048.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                 95.055(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4098(4)
_cell_length_b                   21.0640(5)
_cell_length_c                   18.1097(5)
_cell_measurement_reflns_used    5886
_cell_measurement_temperature    122.97(10)
_cell_measurement_theta_max      73.3930
_cell_measurement_theta_min      4.1860
_cell_volume                     5475.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      122.97(10)
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.947
_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    -19.00  26.00   1.00   60.00    --  -44.92  37.00-150.00   45
  2  \w     -4.00  24.00   1.00   60.00    --  -44.92  19.00 -90.00   28
  3  \w    -15.00  26.00   1.00   60.00    --  -44.92  37.00 -60.00   41
  4  \w     -5.00  30.00   1.00   60.00    --  -44.92  19.00-180.00   35
  5  \w    -18.00  40.00   1.00   60.00    --   44.92 -77.00  30.00   58
  6  \w    105.00 174.00   1.00  190.00    --  103.19 125.00-120.00   69
  7  \w     70.00 168.00   1.00  190.00    --  103.19  15.00 -30.00   98
  8  \w     37.00  72.00   1.00  190.00    --  103.19 -45.00-150.00   35
  9  \w    120.00 175.00   1.00  190.00    --  103.19  77.00-150.00   55
 10  \w     22.00 100.00   1.00  190.00    --  103.19 -94.00-180.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19828
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.426
_diffrn_reflns_theta_min         3.726
_exptl_absorpt_coefficient_mu    4.251
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.091
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         10428
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0346P)^2^+7.4720P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7687
_reflns_number_total             10428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04242a2.cif
_cod_data_source_block           maw219_1m_mp_abs
_cod_depositor_comments
'Adding full bibliography for 1575224--1575230.cif.'
_cod_original_cell_volume        5475.4(2)
_cod_database_code               1575225
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C54.5H75FeMgN2P6
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.698
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C24B-C23B \\sim C24A-C23A \\sim C25B-C23B \\sim C25A-C23A \\sim C23A-C18 \\sim
C23B-C18
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C53 \\sim C54 \\sim C55 \\sim C57 \\sim C56: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
C23B \\sim C23A \\sim C18 \\sim C24B \\sim C24A \\sim C25B \\sim C25A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
4. Others
 Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23B)=Sof(H23B)=Sof(C25B)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25A)=
 Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Fixed Sof: C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C56(0.5) H56A(0.5)
 H56B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C53(0.5)
 H53A(0.5) H53B(0.5) H53C(0.5)
5.a Ternary CH refined with riding coordinates:
 C37(H37), C26(H26), C40(H40), C23A(H23A), C23B(H23B)
5.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C55(H55A,H55B), C54(H54A,H54B)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C15(H15), C8(H8), C2(H2), C19(H19), C20(H20), C21(H21), C12(H12),
 C5(H5), C4(H4), C9(H9), C3(H3), C34(H34), C33(H33), C35(H35), C11(H11),
 C10(H10)
5.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C13(H13A,H13B,H13C), C52(H52A,H52B,H52C), C30(H30A,H30B,
 H30C), C48(H48A,H48B,H48C), C51(H51A,H51B,H51C), C49(H49A,H49B,H49C), C28(H28A,
 H28B,H28C), C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C38(H38A,H38B,H38C),
 C27(H27A,H27B,H27C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C24A(H24A,H24B,
 H24C), C25A(H25A,H25B,H25C), C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F),
 C57(H57A,H57B,H57C), C53(H53A,H53B,H53C)
;
_shelx_res_checksum              25864
_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 1.572
_oxdiff_exptl_absorpt_empirical_full_min 0.718