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_1575224
_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         'C22 H39 Fe Mg O3 P5, 0.55[C4H8O]'
_chemical_formula_sum            'C24 H43 Fe Mg O3.5 P5'
_chemical_formula_weight         622.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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            8
_cell_length_a                   31.9024(4)
_cell_length_b                   11.25500(10)
_cell_length_c                   16.6438(2)
_cell_measurement_reflns_used    8826
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.3600
_cell_measurement_theta_min      4.1380
_cell_volume                     5976.15(12)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 16.8189
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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   -110.00 -25.00   1.00    2.00    --  -45.40 -57.00-120.00   85
  2  \w    -16.00  21.00   1.00    2.00    --  -45.40  37.00-120.00   37
  3  \w     -5.00  20.00   1.00    2.00    --  -45.40  19.00   0.00   25
  4  \w     34.00 102.00   1.00    6.00    --  104.50-125.00 -90.00   68
  5  \w     99.00 164.00   1.00    6.00    --  104.50  61.00-180.00   65
  6  \w     34.00  67.00   1.00    6.00    --  104.50-125.00-150.00   33
  7  \w    105.00 170.00   1.00    6.00    --  104.50 125.00  60.00   65
  8  \w     68.00 141.00   1.00    6.00    --  104.50  15.00 120.00   73
  9  \w     46.00  73.00   1.00    6.00    --  104.50-125.00   0.00   27
 10  \w     77.00 104.00   1.00    6.00    --  104.50-125.00   0.00   27
 11  \w     77.00 102.00   1.00    6.00    --  104.50-125.00-150.00   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  0.0275
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21198
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.403
_diffrn_reflns_theta_min         4.165
_exptl_absorpt_coefficient_mu    6.996
_exptl_absorpt_correction_T_max  0.386
_exptl_absorpt_correction_T_min  0.140
_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 green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.285
_exptl_crystal_size_min          0.233
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         6012
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0366
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+2.4022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5567
_reflns_number_total             6012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc04242a2.cif
_cod_data_source_block           maw303_1mrun1abs
_cod_depositor_comments
'Adding full bibliography for 1575224--1575230.cif.'
_cod_original_formula_sum        'C24 H43 Fe Mg O3.50 P5'
_cod_database_code               1575224
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C25H43FeMgO3P5
_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
2. Restrained distances
 O4-C3 = O4-C6
 1.44 with sigma of 0.02
 C3-C4 = C5-C6
 1.53 with sigma of 0.02
 C4-C5
 1.54 with sigma of 0.02
 O4-C4 = O4-C5 = C3-C5 = C4-C6
 2.38 with sigma of 0.04
 C3-C4 \\sim C4-C5 \\sim C5-C6
 with sigma of 0.02
 O4-C3 \\sim O4-C6
 with sigma of 0.02
 O4-C4 \\sim O4-C5
 with sigma of 0.04
 C4-C6 \\sim C3-C5
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O4 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
4. Rigid body (RIGU) restrains
 O4, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O4(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5)
 C5(0.5) H5A(0.5) H5B(0.5) C6(0.5) H6A(0.5) H6B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00H(H00C,H00D), C00I(H00E,H00F), C00J(H00G,H00H), C00K(H00I,
 H00J), C00M(H00N,H00O), C00N(H00P,H00Q), C00O(H00R,H00S), C00R(H00Z,H),
 C00U(H2,HE), C00V(H3,HF), C00W(H4,HG), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
 C6(H6A,H6B)
6.b Idealised Me refined as rotating group:
 C00L(H00K,H00L,H00M), C00P(H00T,H00U,H00V), C00Q(H00W,H00X,H00Y), C00S(H00,HA,
 HB), C00T(H1,HC,HD)
;
_shelx_res_checksum              22525
_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.760