Synthesis, Crystal Structure, and Relativistic DV-Xα Calculation of a μ-Oxido-μ-molybdato(VI)-bridged Dinuclear Oxidomolybdenum(V) Complex with 2-(3-Aminopropyl)aminoethanethiol
MIKURIYA, Masahiro; KUSUNOKI, Koji; KOTERA, Takanori; YOSHIOKA, Daisuke; TAKEMURA, Shota; OGASAWARA, Kazuyoshi; X-ray Structure Analysis Online 34 (2018) 19–; doi:10.2116/xraystruct.34.19

data_1551566
_publ_section_title
;
 Synthesis, Crystal Structure, and Relativistic DV-X\a Calculation of a
 \m-Oxido-\m-molybdato(VI)-bridged Dinuclear Oxidomolybdenum(V) Complex
 with 2-(3-Aminopropyl)aminoethanethiol
;
_journal_issue                   0
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              19
_journal_paper_doi               10.2116/xraystruct.34.19
_journal_volume                  34
_journal_year                    2018
_chemical_formula_sum            'C12 H34 Mo3 N4 O9 S2'
_chemical_formula_weight         730.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.192(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.558(3)
_cell_length_b                   8.9725(13)
_cell_length_c                   17.193(3)
_cell_measurement_reflns_used    15957
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.933
_cell_measurement_theta_min      2.369
_cell_volume                     2554.3(7)
_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 0.911
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15957
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.933
_diffrn_reflns_theta_min         2.369
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.659
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            reddish-brown
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_description       needle
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0309P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0768
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5032
_reflns_number_total             6166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            34_19_1.txt
_cod_data_source_block           Mof5kk1m_0m
_cod_database_code               1551566
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.636
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              32835
_shelx_hkl_checksum              13963