Synthesis and Crystal Structure of a Tetranuclear Oxidovanadium(IV) Complex with 2,6-Bis(hydroxymethyl)-4-methylphenol
MIKURIYA, Masahiro; FUKUTANI, Masami; OMOTE, Masataka; YOSHIOKA, Daisuke; MITSUHASHI, Ryoji; X-ray Structure Analysis Online 32 (2016) 15–; doi:10.2116/xraystruct.32.15

data_1551603
_publ_section_title
;
 Synthesis and Crystal Structure of a Tetranuclear Oxidovanadium(IV)
 Complex with 2,6-Bis(hydroxymethyl)-4-methylphenol
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              15
_journal_paper_doi               10.2116/xraystruct.32.15
_journal_volume                  32
_journal_year                    2016
_chemical_formula_sum            'C34 H62 N2 O20 S2 V4'
_chemical_formula_weight         1086.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                109.294(9)
_cell_angle_beta                 114.158(7)
_cell_angle_gamma                102.452(9)
_cell_formula_units_Z            1
_cell_length_a                   10.799(5)
_cell_length_b                   11.339(5)
_cell_length_c                   11.703(5)
_cell_measurement_reflns_used    7044
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.534
_cell_measurement_theta_min      2.371
_cell_volume                     1127.0(9)
_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 0.990
_diffrn_measured_fraction_theta_max 0.881
_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  0.0292
_diffrn_reflns_av_unetI/netI     0.0955
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7044
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.534
_diffrn_reflns_theta_min         2.371
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.975
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0548
_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^)+(0.0367P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1126
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3630
_reflns_number_total             5060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            32_15_1.txt
_cod_data_source_block           ydkr_a
_cod_original_cell_volume        1127.0(8)
_cod_database_code               1551603
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              13464
_shelx_hkl_checksum              41753