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_1575230
_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(C11 H18 Fe P5), C12 H30 Mg O6, C4 H10 O2'
_chemical_formula_sum            'C38 H76 Fe2 Mg O8 P10'
_chemical_formula_weight         1106.69
_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                 95.224(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5512(6)
_cell_length_b                   14.2205(7)
_cell_length_c                   37.349(2)
_cell_measurement_reflns_used    5897
_cell_measurement_temperature    122.98(11)
_cell_measurement_theta_max      71.3500
_cell_measurement_theta_min      3.2780
_cell_volume                     5580.7(5)
_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 1.5-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      122.98(11)
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.970
_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   -121.00 -25.00   1.00   17.50    --  -43.14 -19.00-120.00   96
  2  \w      7.00  34.00   1.00   17.50    --  -43.14  19.00-180.00   27
  3  \w    -14.00  23.00   1.00   17.50    --  -43.14  38.00-150.00   37
  4  \w     62.00 110.00   1.00   17.50    --   43.14 178.00-120.00   48
  5  \w     97.00 160.00   1.00  140.00    --  104.50 125.00 150.00   63
  6  \w     31.00  56.00   1.00  140.00    --  104.50 -30.00  90.00   25
  7  \w     31.00  57.00   1.00  140.00    --  104.50 -30.00 120.00   26
  8  \w    105.00 173.00   1.00  140.00    --  104.50  77.00  30.00   68
  9  \w     35.00  67.00   1.00  140.00    --  104.50 -45.00 150.00   32
 10  \w     34.00  59.00   1.00  140.00    --  104.50 -45.00 120.00   25
 11  \w     31.00  56.00   1.00  140.00    --  104.50 -30.00-120.00   25
 12  \w     41.00  68.00   1.00  140.00    --  104.50 -45.00   0.00   27
 13  \w     51.00  77.00   1.00  140.00    --  104.50 -61.00-180.00   26
 14  \w     41.00  71.00   1.00  140.00    --  104.50 -45.00 -60.00   30
 15  \w     34.00 125.00   1.00  140.00    --  104.50 -77.00  90.00   91
 16  \w     36.00  68.00   1.00  140.00    --  104.50 -45.00 -90.00   32
 17  \w     31.00  56.00   1.00  140.00    --  104.50 -30.00  30.00   25
;
_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  0.0670
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            24832
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.069
_diffrn_reflns_theta_min         2.376
_exptl_absorpt_coefficient_mu    7.333
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.198
_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    1.317
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.142
_exptl_crystal_size_min          0.127
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.00010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         10987
_refine_ls_number_restraints     526
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+2.1736P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2191
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7378
_reflns_number_total             10987
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04242a2.cif
_cod_data_source_block           maw296_1mrun1abs
_cod_depositor_comments
'Adding full bibliography for 1575224--1575230.cif.'
_cod_database_code               1575230
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C38H73Fe2MgO8P10
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 P8-C18 \\sim P13-C18
 with sigma of 0.04
 P9-C18 \\sim P14-C18
 with sigma of 0.02
 P10-C18 \\sim P15-C18
 with sigma of 0.04
 P7-P6 \\sim P12-P11
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C4 \\sim C7 \\sim C11 \\sim C12 \\sim C27 \\sim C30 \\sim C35
\\sim C37 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45
\\sim C46 \\sim C47 \\sim C48: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C3 \\sim C5 \\sim C6 \\sim C9 \\sim C17 \\sim C21 \\sim C31 \\sim C32 \\sim C34
\\sim C36 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55
\\sim C56 \\sim C57 \\sim C58: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
Uanis(C44) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(P11)=Sof(P12)=Sof(P13)=Sof(P14)=Sof(P15)=1-
 FVAR(1)
 Sof(P6)=Sof(P7)=Sof(P8)=Sof(P9)=Sof(P10)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(1)
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(C41)=Sof(C42)=Sof(C43)=
 Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=Sof(C45)=
 Sof(C46)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 Sof(H48C)=1-FVAR(2)
 Sof(C1)=Sof(C2)=Sof(C4)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C11)=Sof(C12)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=
 FVAR(2)
 Sof(C50)=Sof(C54)=Sof(C49)=Sof(C52)=Sof(C51)=Sof(C53)=Sof(H53A)=Sof(H53B)=
 Sof(H53C)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(H55C)=Sof(C56)=Sof(H56A)=Sof(H56B)=
 Sof(H56C)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=Sof(H58B)=
 Sof(H58C)=1-FVAR(3)
 Sof(C3)=Sof(C5)=Sof(C6)=Sof(C9)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(C21)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C36)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C16(H16A,H16B), C19(H19A,H19B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B)
5.b Fitted pentagon refined as free rotating group:
 C50(C54,C49,C52,C51)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18D,H18E,H18F), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C27(H27A,
 H27B,H27C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C)
;
_shelx_res_checksum              29635
_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 2.599
_oxdiff_exptl_absorpt_empirical_full_min 0.519