Synthesis, crystal structure and selected properties of two new peroxidomolybdates
Sławińska, Adrianna; Serda, Paweł; Oszajca, Marcin; Pamin, Katarzyna; Połtowicz, Jan; Łasocha, Wiesław; Polyhedron 183 (2020) 114530–; doi:10.1016/j.poly.2020.114530

data_1566070
_publ_section_title
;
 Synthesis, crystal structure and selected properties of two new
 peroxidomolybdates
;
_journal_name_full               Polyhedron
_journal_page_first              114530
_journal_paper_doi               10.1016/j.poly.2020.114530
_journal_volume                  183
_journal_year                    2020
_chemical_formula_moiety         'C12 H8 Mo2 N2 O16, 2(H2 O), 2(H4 N)'
_chemical_formula_sum            'C12 H20 Mo2 N4 O18'
_chemical_formula_weight         700.20
_chemical_name_systematic
'Diammonium [tetrakis(\h2-peroxido)dioxido-bis{\m-(1-oxo-\kO-pyridine-4-carboxylate-\kO)}dimolybdate(VI) dihydrate'
_chemical_properties_physical    Heat-sensitive
_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   mixed
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                91.517(3)
_cell_angle_beta                 96.093(3)
_cell_angle_gamma                104.610(4)
_cell_formula_units_Z            1
_cell_length_a                   6.5619(3)
_cell_length_b                   7.1063(3)
_cell_length_c                   12.0469(4)
_cell_measurement_reflns_used    8421
_cell_measurement_temperature    131(2)
_cell_measurement_theta_max      76.7771
_cell_measurement_theta_min      3.6925
_cell_volume                     539.69(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      131(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9628
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.980
_diffrn_reflns_theta_min         3.696
_exptl_absorpt_coefficient_mu    10.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_description       plate
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.131
_refine_diff_density_min         -1.605
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2241
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+1.0437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2205
_reflns_number_total             2241
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Poly-2020-183-114530.cif
_cod_data_source_block           2
_cod_database_code               1566070
_shelx_estimated_absorpt_t_min   0.207
_shelx_estimated_absorpt_t_max   0.623
_shelxl_version_number           2013-4
_shelx_res_checksum              6739
_shelx_hkl_checksum              52553