Synthesis and Structural Elucidation of Triazolylmolybdenum(VI) Oxide Hybrids and Their Behavior as Oxidation Catalysts.
Lysenko, Andrey B.; Senchyk, Ganna A.; Domasevitch, Konstantin V.; Hauser, Jürg; Fuhrmann, Daniel; Kobalz, Merten; Krautscheid, Harald; Neves, Patrícia; Valente, Anabela A.; Gonçalves, Isabel S; Inorganic chemistry 54 (2015) 8327–8338; doi:10.1021/acs.inorgchem.5b01007

data_4346222
_publ_section_title
;
 Synthesis and Structural Elucidation of Triazolylmolybdenum(VI) Oxide
 Hybrids and Their Behavior as Oxidation Catalysts.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8327
_journal_page_last               8338
_journal_paper_doi               10.1021/acs.inorgchem.5b01007
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C7 H13 Mo2 N5 O8'
_chemical_formula_sum            'C7 H13 Mo2 N5 O8'
_chemical_formula_weight         487.1
_chemical_name_systematic
;
poly[di-\m-oxido-\m-
[4-[3,5-dimethylpyrazol-4-yl]-4H-1,2,4-triazole-
\k^4^N1:N2]-diaqua-tetraoxodimolybdenum(VI)]

;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 99.2369(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.71946(6)
_cell_length_b                   20.35701(13)
_cell_length_c                   9.41202(9)
_cell_measurement_reflns_used    19258
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      31.572
_cell_measurement_theta_min      1.994
_cell_volume                     1459.87(2)
_computing_cell_refinement
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
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_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
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        (compiled Aug  2 2013,16:46:58)
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_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
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_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16.0965
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.037672
_diffrn_orient_matrix_UB_12      0.0312091
_diffrn_orient_matrix_UB_13      -0.0188763
_diffrn_orient_matrix_UB_21      0.060763
_diffrn_orient_matrix_UB_22      0.0147823
_diffrn_orient_matrix_UB_23      0.0553043
_diffrn_orient_matrix_UB_31      0.0596161
_diffrn_orient_matrix_UB_32      0.0046499
_diffrn_orient_matrix_UB_33      -0.0491411
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            31977
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.901
_diffrn_reflns_theta_min         2.001
_exptl_absorpt_coefficient_mu    1.766
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.57315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       rod
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.0487
_exptl_crystal_size_min          0.0264
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.651
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4805
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0152P)^2^+1.3143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0433
_reflns_number_gt                4402
_reflns_number_total             4805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01007_si_002.cif
_cod_data_source_block           (2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346222