Syntheses and crystal structures of new naphthalene– and anthracene–vanadate salts and an unprecedented dimetallabis(anthracene) sandwich complex: [Na(tetrahydrofuran)~3~][V~2~(anthracene)~2~]
Kucera, Benjamin E.; Young, Jr, Victor G.; Brennessel, William W.; Ellis, John E.; Acta Crystallographica Section C 78 (2022) –; doi:10.1107/S2053229622001255

data_2022537
_publ_section_title
;
 Syntheses and crystal structures of new naphthalene-- and
 anthracene--vanadate salts and an unprecedented dimetallabis(anthracene)
 sandwich complex: [Na(tetrahydrofuran)~3~][V~2~(anthracene)~2~]
;
_journal_coeditor_code           ZO3016
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229622001255
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac
;
[K (C12 H24 O6) (C4 H8 O1)2] [K V2 (C12 H24 O6) (C4 H8 O1)2 (C14 H10)4],
2C4 H8 O
;
_chemical_formula_moiety         'C76 H80 K O8 V2, C20 H40 K O8, 2(C4 H8 O)'
_chemical_formula_sum            'C104 H136 K2 O18 V2'
_chemical_formula_weight         1854.20
_chemical_name_systematic
;(1,4,7,10,13,16-Hexaoxacyclooctadecane)bis(tetrahydrofuran)potassium
[(\h^4^-anthracene)(tetrahydrofuran)vanadium]-\m-\h^4^:\h^2^-anthracene-[(1,4,7,10,13,16-Hexaoxacyclooctadecane)potassium]-\m-\h^2^:\h^4^-anthracene-[(\h^4^-anthracene)(tetrahydrofuran)vanadium] tetrahydrofuran disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                89.695(3)
_cell_angle_beta                 88.670(3)
_cell_angle_gamma                83.918(4)
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_cell_length_a                   9.1729(16)
_cell_length_b                   9.3501(16)
_cell_length_c                   27.928(5)
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_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.10
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_computing_cell_refinement
;
SAINT (Bruker, 2003)
;
_computing_data_collection
;
SMART (Bruker, 2003)
;
_computing_data_reduction
;
SAINT (Bruker, 2003)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
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;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens SMART CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0654
_diffrn_reflns_av_unetI/netI     0.0945
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            21602
_diffrn_reflns_theta_full        25.096
_diffrn_reflns_theta_max         25.096
_diffrn_reflns_theta_min         1.459
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  0.9826
_exptl_absorpt_correction_T_min  0.9019
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.359
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         8389
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0534
_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^)+(0.0338P)^2^+1.6334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1222
_reflns_number_gt                4713
_reflns_number_total             8389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3016sup1.cif
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_shelx_estimated_absorpt_t_min   0.902
_shelx_estimated_absorpt_t_max   0.983
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_cod_database_fobs_code 2022537