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_2022535
_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          '[K2 V (C4 H8 O)4 (C10 H8)2]'
_chemical_formula_moiety         '2(C8 H16 O2 K), C20 H16 V'
_chemical_formula_sum            'C36 H48 K2 O4 V'
_chemical_formula_weight         673.88
_chemical_name_systematic
<i>catena</i>-Poly[bis(\m-~3~\h^4^:\h^6^:\h^4^-naphthalene)tetrakis(tetrahydrofuran)dipotassiumvanadium]
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 101.014(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.985(2)
_cell_length_b                   17.243(4)
_cell_length_c                   18.532(4)
_cell_measurement_reflns_used    3155
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.33
_cell_volume                     3445.6(13)
_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
;
SHELXS-97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27058
_diffrn_reflns_theta_full        25.085
_diffrn_reflns_theta_max         25.085
_diffrn_reflns_theta_min         1.627
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  0.8952
_exptl_absorpt_correction_T_min  0.7651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       rod
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         6104
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0525P)^2^+1.6694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1061
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                4007
_reflns_number_total             6104
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3016sup1.cif
_cod_data_source_block           3
_cod_original_cell_volume        3445.5(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2022535
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.895
_shelx_hkl_checksum              37638
_shelx_res_checksum              39864
_cod_database_fobs_code 2022535