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_2022536
_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_absolute_configuration ad
_chemical_formula_iupac
'[K (C18 H36 N2 O6)] [V (C10 H8)2 (C6 H16 P2)], C4 H8 O'
_chemical_formula_moiety         'C18 H36 K N2 O6 +, C26 H32 P2 V -, C4 H8 O'
_chemical_formula_sum            'C48 H76 K N2 O7 P2 V'
_chemical_formula_weight         945.08
_chemical_name_common
;([2.2.2]Cryptand)potassium
[1,2-bis(dimethylphosphanyl)ethane]bis(\h^4^-naphthalene)vanadium
tetrahydrofuran
;
_chemical_name_systematic
;(4,7,13,16,21,24-Hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane)potassium
[1,2-bis(dimethylphosphanyl)ethane]bis(naphthalene)vanadium tetrahydrofuran
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           3
_space_group_name_Hall           'P 2y'
_space_group_name_H-M_alt        'P 1 2 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                 108.835(2)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   10.3028(11)
_cell_length_b                   8.6409(9)
_cell_length_c                   14.5778(15)
_cell_measurement_reflns_used    2618
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.55
_cell_measurement_theta_min      2.36
_cell_volume                     1228.3(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0483
_diffrn_reflns_av_unetI/netI     0.0709
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10165
_diffrn_reflns_theta_full        25.085
_diffrn_reflns_theta_max         25.085
_diffrn_reflns_theta_min         1.476
_diffrn_source                   'normal-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.402
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_correction_T_min  0.9062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       plate
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.279
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1372 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4352
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.0452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                3491
_reflns_number_total             4352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zo3016sup1.cif
_cod_data_source_block           4b
_cod_original_sg_symbol_H-M      'P 2'
_cod_database_code               2022536
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_checksum              10698
_shelx_res_checksum              93405
_cod_database_fobs_code 2022536