Synthesis and Crystal Structure of Another Tetranuclear Oxidovanadium(IV) Complex with 2,6-Bis(hydroxymethyl)-4-methylphenol Having an N<sub>2</sub>-Adsorption Property
MIKURIYA, Masahiro; FUKUTANI, Masami; OMOTE, Masataka; YOSHIOKA, Daisuke; MITSUHASHI, Ryoji; TANAKA, Hidekazu; HANDA, Makoto; X-ray Structure Analysis Online 32 (2016) 29–; doi:10.2116/xraystruct.32.29

data_1551618
_publ_section_title
;
 Synthesis and Crystal Structure of Another Tetranuclear Oxidovanadium(IV)
 Complex with 2,6-Bis(hydroxymethyl)-4-methylphenol Having an
 N&lt;sub&gt;2&lt;/sub&gt;-Adsorption Property
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              29
_journal_paper_doi               10.2116/xraystruct.32.29
_journal_volume                  32
_journal_year                    2016
_chemical_formula_sum            'C34 H64 N2 O21 S2 V4'
_chemical_formula_weight         1104.75
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.000(4)
_cell_angle_beta                 90.000(4)
_cell_angle_gamma                120.000(3)
_cell_formula_units_Z            18
_cell_length_a                   45.690(8)
_cell_length_b                   45.690(8)
_cell_length_c                   12.589(2)
_cell_measurement_reflns_used    47923
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.677
_cell_measurement_theta_min      2.115
_cell_volume                     22760(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0881
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       61
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            47923
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.677
_diffrn_reflns_theta_min         2.115
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       needle
_exptl_crystal_F_000             10332
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         12145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0614
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7887
_reflns_number_total             12145
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            32_29_1.txt
_cod_data_source_block           VMO06
_cod_original_cell_volume        22758(9)
_cod_database_code               1551618
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.880
_shelx_res_checksum              85880
_shelx_hkl_checksum              83480
_shelx_fab_checksum              56459