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_1575228
_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         'C70 H104 Fe2 O6 P12 Sr2, 2(C4 H8 O)'
_chemical_formula_sum            'C78 H120 Fe2 O8 P12 Sr2'
_chemical_formula_weight         1844.31
_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                 90.3120(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.7954(2)
_cell_length_b                   20.3376(3)
_cell_length_c                   19.5093(3)
_cell_measurement_reflns_used    8474
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      64.9440
_cell_measurement_theta_min      3.1240
_cell_volume                     4283.25(12)
_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      123.01(10)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_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     63.00 106.00   0.50    2.00    --   62.53  15.00-150.00   86
  2  \w     92.00 118.00   0.50    2.00    --   79.75  43.00-165.63   52
  3  \w    -72.00 -41.00   0.50    2.00    --  -78.25  73.00  46.85   62
  4  \w   -115.00 -87.00   0.50    2.00    --  -78.25 -71.00   7.09   56
  5  \w   -112.00 -85.00   0.50    2.00    --  -78.25 -80.00 147.04   54
  6  \w     25.00  66.00   0.50    2.00    --   62.53   0.00 -30.00   82
  7  \w     49.00 124.00   0.50    2.00    --   79.75  11.00-168.12  150
  8  \w     31.00  60.00   0.50    2.00    --   62.53  15.00-150.00   58
  9  \w     75.00 100.00   0.50    2.00    --   62.53   0.00 -30.00   50
 10  \w     50.00 123.00   0.50    2.00    --   79.75  11.00 103.44  146
 11  \w     42.00  80.00   0.50    2.00    --   79.75  -4.00 110.97   76
 12  \w     33.00  68.00   0.50    2.00    --   62.53 -95.00  30.00   70
 13  \w     26.00  61.00   0.50    2.00    --   62.53 -95.00-150.00   70
 14  \w     39.00  90.00   0.50    2.00    --   79.75-105.00-175.26  102
;
_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  0.0624
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19761
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        65.130
_diffrn_reflns_theta_max         65.130
_diffrn_reflns_theta_min         3.139
_exptl_absorpt_coefficient_mu    6.774
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.515
_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 dark red'
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       needle
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         6955
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0886P)^2^+0.1126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1380
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5594
_reflns_number_total             6955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04242a2.cif
_cod_data_source_block           maw460_1m_red2abs
_cod_depositor_comments
'Adding full bibliography for 1575224--1575230.cif.'
_cod_database_code               1575228
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C78H118.5Fe2O7.5P12Sr2
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.375
_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
 O4-C36 \\sim O5-C40
 with sigma of 0.02
 O4-C39 \\sim O5-C43
 with sigma of 0.02
 C37-C39 \\sim C41-C43
 with sigma of 0.04
 C36-C38 \\sim C40-C42
 with sigma of 0.04
 C36-C37 \\sim C40-C41
 with sigma of 0.02
 C37-C38 \\sim C41-C42
 with sigma of 0.02
 C36-C39 \\sim C40-C43
 with sigma of 0.04
 C38-C39 \\sim C42-C43
 with sigma of 0.02
 O4-C37 \\sim O5-C41
 with sigma of 0.04
 O4-C38 \\sim O5-C42
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O4 \\sim C36 \\sim C37 \\sim C38 \\sim C39: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
O4 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim O5 \\sim C40 \\sim C41 \\sim
C42 \\sim C43: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Others
 Sof(O5)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=
 Sof(H42A)=Sof(H42B)=Sof(C43)=Sof(H43A)=Sof(H43B)=1-FVAR(1)
 Sof(O4)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=
 Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B)
5.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16),
 C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              74451
_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 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.768