Synthesis and characterization of asymmetric [Mo2O2(μ-S)2(S2)(L)] complexes (L = bipy, en, dien) and their heterogeneous reaction with propylene sulfide
Birgisson, Benedikt O.; Monger, Lindsey J.; Damodaran, Krishna K.; Suman, Sigridur G.; Inorganica Chimica Acta 501 (2020) 119272–; doi:10.1016/j.ica.2019.119272

data_1565616
_publ_section_title
;
 Synthesis and characterization of asymmetric [Mo2O2(\m-S)2(S2)(L)]
 complexes (L&#x202F;=&#x202F;bipy, en, dien) and their heterogeneous
 reaction with propylene sulfide
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119272
_journal_paper_doi               10.1016/j.ica.2019.119272
_journal_volume                  501
_journal_year                    2020
_chemical_formula_moiety         'C13 H15 Mo2 N3 O3 S4'
_chemical_formula_sum            'C13 H15 Mo2 N3 O3 S4'
_chemical_formula_weight         581.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                69.4630(10)
_cell_angle_beta                 84.0190(10)
_cell_angle_gamma                60.9330(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6507(3)
_cell_length_b                   9.6875(4)
_cell_length_c                   12.4793(5)
_cell_measurement_reflns_used    9885
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.10
_cell_volume                     951.82(6)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_collection       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_computing_molecular_graphics    'MERCURY CSD 3.8'
_computing_publication_material  'MERCURY CSD 3.8'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SAINT V8.35A (?, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0127
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27669
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         3.101
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Multi-scan was used for absorption correction. wR2(int) was 0.0457 before and 0.0387 after correction. The Ratio of minimum to maximum transmission is 0.9071. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_description       plate
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0177
_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^)+(0.0199P)^2^+1.1136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0438
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3187
_reflns_number_total             3496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-501-119272.cif
_cod_data_source_block           mo_SSBOB269_0m
_cod_database_code               1565616
_shelx_estimated_absorpt_t_min   0.707
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              99934
_shelx_hkl_checksum              46852