Synthesis, Crystal Structure, and DFT Calculation of a Dioxido-bridged Dinuclear Oxidomolybdenum(V) Complex with 2-(2-Aminoethyl)aminoethanethiol
MIKURIYA, Masahiro; KUSUNOKI, Koji; KOTERA, Takanori; YOSHIOKA, Daisuke; OGASAWARA, Kazuyoshi; X-ray Structure Analysis Online 33 (2017) 37–; doi:10.2116/xraystruct.33.37

data_1551591
_publ_section_title
;
 Synthesis, Crystal Structure, and DFT Calculation of a Dioxido-bridged
 Dinuclear Oxidomolybdenum(V) Complex with
 2-(2-Aminoethyl)aminoethanethiol
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              37
_journal_paper_doi               10.2116/xraystruct.33.37
_journal_volume                  33
_journal_year                    2017
_chemical_formula_sum            'C8 H22 Mo2 N4 O4 S2'
_chemical_formula_weight         494.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.091(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.975(3)
_cell_length_b                   12.475(3)
_cell_length_c                   12.158(3)
_cell_measurement_reflns_used    2384
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.456
_cell_measurement_theta_min      2.204
_cell_volume                     2086.8(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.901
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.456
_diffrn_reflns_theta_min         2.204
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.765
_exptl_absorpt_correction_T_min  0.538
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            reddish-brown?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0561P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1617
_reflns_number_total             2384
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            33_37_1.txt
_cod_data_source_block           ydkr
_cod_database_code               1551591
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.538
_shelx_estimated_absorpt_t_max   0.765
_shelx_res_checksum              37726
_shelx_hkl_checksum              23743
_shelx_fab_checksum              69140