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_2022538
_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 (C20 H40 O8)] [V (C14 H10)2 (C3 H9 P)], C4 H8 O'
_chemical_formula_moiety         'C20 H40 K O8, C31 H29 P V, C4 H8 O'
_chemical_formula_sum            'C55 H77 K O9 P V'
_chemical_formula_weight         1003.17
_chemical_name_common
;(18-Crown-6)bis(tetrahydrofuran)potassium
bis(\h^4^-anthracene)(trimethylphosphane)vanadium tetrahydrofuran monosolvate
;
_chemical_name_systematic
;(1,4,7,10,13,16-Hexaoxacyclooctadecane)bis(tetrahydrofuran)potassium bis(\h^4^-anthracene)(trimethylphosphane)vanadium
tetrahydrofuran monosolvate
;
_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                74.992(2)
_cell_angle_beta                 84.667(2)
_cell_angle_gamma                71.815(2)
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_cell_length_a                   9.6431(12)
_cell_length_b                   14.4883(18)
_cell_length_c                   20.804(3)
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_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
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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)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      173(2)
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_diffrn_measured_fraction_theta_max 0.986
_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  0.0387
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_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23058
_diffrn_reflns_theta_full        25.051
_diffrn_reflns_theta_max         25.051
_diffrn_reflns_theta_min         1.525
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.9338
_exptl_absorpt_correction_T_min  0.8735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.424
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         9330
_refine_ls_number_restraints     409
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0537
_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^)+(0.0392P)^2^+2.0007P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1175
_reflns_number_gt                6704
_reflns_number_total             9330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3016sup1.cif
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_shelx_estimated_absorpt_t_min   0.874
_shelx_estimated_absorpt_t_max   0.934
_shelx_hkl_checksum              73447
_shelx_res_checksum              5992
_cod_database_fobs_code 2022538