Crystal structure of (μ-hydrogen di-sulfato)-μ-oxido-bis-[(4,4'-di-<i>tert</i>-butyl-2,2'-bi-pyridine)-oxidovanadium(IV/V)] aceto-nitrile monosolvate.
Kodama, Shintaro; Hashiguchi, Terushi; Nomoto, Akihiro; Acta crystallographica. Section E, Crystallographic communications 79 (2023) 1055–1058; doi:10.1107/S2056989023009040

data_2022920
_publ_section_title
;
 Crystal structure of (&#x3bc;-hydrogen
 di-sulfato)-&#x3bc;-oxido-bis-[(4,4'-di-<i>tert</i>-butyl-2,2'-bi-pyridine)-oxidovanadium(IV/V)]
 aceto-nitrile monosolvate.
;
_journal_coeditor_code           NX2001
_journal_issue                   'Pt 11'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1055
_journal_page_last               1058
_journal_paper_doi               10.1107/S2056989023009040
_journal_volume                  79
_journal_year                    2023
_chemical_formula_iupac          '[V2 (H S2 O8) O3 (C18 H24 N2)2], C2 H3 N'
_chemical_formula_moiety         'C36 H49 N4 O11 S2 V2, C2 H3 N'
_chemical_formula_sum            'C38 H52 N5 O11 S2 V2'
_chemical_formula_weight         920.84
_chemical_name_systematic
;(\m-Hydrogen disulfato)-\m-oxido-bis[(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine)oxidovanadium(IV/V)]
acetonitrile monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.0134(2)
_cell_length_b                   34.9495(5)
_cell_length_c                   39.4864(6)
_cell_measurement_reflns_used    30626
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.5730
_cell_measurement_theta_min      1.8790
_cell_volume                     17958.9(5)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_collection
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CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
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CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
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Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
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Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
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_computing_structure_refinement
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<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
<i>olex2.solve</i> 1.5 (Bourhis et al., 2015)
;
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            51528
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.513
_diffrn_reflns_theta_min         2.063
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2020)
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       Block
_exptl_crystal_F_000             7696
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6582
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.129
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0469P)^2^+46.6480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1054
_refine_ls_wR_factor_ref         0.1101
_reflns_number_gt                5675
_reflns_number_total             6582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            nx2001sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2022920.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               2022920
_cod_database_fobs_code          2022920
_shelx_hkl_checksum              20546
_shelx_res_checksum              89215