Tris(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine)(<i>trans</i>-4-<i>tert</i>-butylcyclohexanolato)deca-μ-oxido-heptaoxidoheptavanadium acetonitrile monosolvate including another unknown solvent molecule
Kodama, Shintaro; Kondo, Shota; Nomoto, Akihiro; Ogawa, Akiya; IUCrData 5 (2020) x200449–; doi:10.1107/S2414314620004496

data_1557751
_publ_section_title
;
 Tris(4,4'-di-<i>tert</i>-butyl-2,2'-bipyridine)(<i>trans</i>-4-<i>tert</i>-butylcyclohexanolato)deca-\m-oxido-heptaoxidoheptavanadium
 acetonitrile monosolvate including another unknown solvent molecule
;
_journal_coeditor_code           IS4043
_journal_issue                   4
_journal_name_full               IUCrData
_journal_page_first              x200449
_journal_paper_doi               10.1107/S2414314620004496
_journal_volume                  5
_journal_year                    2020
_chemical_formula_iupac          '[V7 (C10 H19 O) O17 (C18 H24 N2)3], C2 H3 N'
_chemical_formula_moiety         'C64 H91 N6 O18 V7, C2 H3 N'
_chemical_formula_sum            'C66 H94 N7 O18 V7'
_chemical_formula_weight         1630.10
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.548(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   14.6285(4)
_cell_length_b                   29.9816(7)
_cell_length_c                   20.5191(5)
_cell_measurement_reflns_used    76498
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      1.78
_cell_volume                     8971.0(4)
_computing_cell_refinement
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_collection
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_data_reduction
;
<i>RAPID-AUTO</i> (Rigaku, 2006)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2018)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2018)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1126
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            122082
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.268
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3376.00
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.26
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     905
_refine_ls_number_reflns         16426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0738
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0880P)^2^+32.1684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2017
_reflns_number_gt                12218
_reflns_number_total             16426
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            is4043sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        8971.1(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1557751
_cod_database_fobs_code          1557751
_shelx_hkl_checksum              98130
_shelx_res_checksum              12200
_shelx_fab_checksum              21766